Tag: M.W=300-400

915095-86-2, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 915095-86-2, name is (2-Chloro-5-iodophenyl)(4-fluorophenyl)methanone, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a stirred solution of 1 (0.01 mol) in 30 mL of CH2Cl2and 30 mL of CH3CN at 0 ¡ãC were added Et3SiH(4.79 mL,0.03 mol), then BF3¡¤Et2O(2.53 mL, 0.02 mol), and theresulting mixture was warmed to room temperature andstirred for 3?8 h. The mixture was poured into saturatedaqueous NaHCO3 and extracted with CH2Cl2 twice. Thecombined organic layers were washed with brine, dried overMgSO4, and concentrated. The residual solid was crystallizedfrom ethanol to give as white solid.According to this procedure the following compoundswere prepared. 1-chloro-2-(4-fluorobenzyl)-4-iodobenzene (2a)White solid, yield 83percent, m.p. 52?54 ¡ãC. 1H NMR (400MHz, DMSO-d6): delta 4.02(s, 2H), 7.10?7.13(m, 2H), 7.22?7.25(m, 3H), 7.60(dd, J = 0.8, 6.8 Hz, 1H), 7.72(d, J = 0.8Hz, 1H). 13C NMR (100 MHz, DMSO-d6): delta 36.94, 92.85,115.21(d, J = 68 Hz), 130.30(d, J = 24 Hz), 131.32,133.16, 134.87, 136.82, 139.44, 140.77, 159.80, 161.73.

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Reference:
Article; Hu, Shengquan; Sun, Wuji; Wang, Yeming; Yan, Hong; Medicinal Chemistry Research; vol. 28; 4; (2019); p. 465 – 472;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

628-21-7, The chemical industry reduces the impact on the environment during synthesis 628-21-7, name is 1,4-Diiodobutane, I believe this compound will play a more active role in future production and life.

Sodium hydride (2.8 g, 60% dispersion in mineral oil) was added slowly to a solution of (4-nitro-phenyl)-acetic acid methyl ester (6.0 g, 30.7 mmol) in anhydrous DMF (30 mL) under nitrogen at a temperature in the range of 0 C. to 10 C. After stirring at a temperature in the range of 0 C. to 10 C. for 20 min, diiodobutane (7.86 mL, 61 mmol) was added drop-wise under stirring. After complete addition, the reaction mixture was warmed to a temperature in the range of 15 C. to 40 C. and stirring continued for an additional 3 hours. The reaction was quenched by adding water slowly. The mixture was extracted by ethyl acetate (3¡Á40 mL). The combined organic extracts were washed with water, brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The resultant gummy material was purified by column chromatography over silica gel to afford a pale yellow thick liquid which solidified on standing at a temperature in the range of 15 C. to 40 C. (4.1 g, 54% yield). The solid (3.4 g, 13.6 mmol) was dissolved in anhydrous EtOH and tin chloride dihydrate (13.86 g, 61 mmol) was added slowly under nitrogen. Thereafter, the mixture was heated at 90 C. for 3 hours. After evaporation of volatiles under reduced pressure, the resultant mixture was diluted with ice-water and aqueous sodium hydroxide was added to adjust pH 11. The mixture was extracted with ethyl acetate (3¡Á50 mL). The combined organic extracts were washed with water, brine, dried over Na2SO4, filtered, and the filtrate was concentrated under reduced pressure to afford the title compound as a granular light yellow solid (2.67 g, 88% yield).1HNMR (CDCl3, 300 MHz): delta 7.16 (dd, J=8.4, 1.8 Hz, 2H), 6.63 (dd, J=8.4, 1.8 Hz, 2H), 3.59 (s, 3H), 2.60-2.55 (m, 2H), 1.87-1.67 (m, 6H).LC-MSD (ES+): (m/z) 220 [(M+H)+, 100].

The chemical industry reduces the impact on the environment during synthesis 628-21-7. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Dr. Reddy’s Laboratories Ltd.; US2010/144731; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common compound: 3268-21-1, name is 1,4-Diiodo-2,3,5,6-tetramethylbenzene, belongs to iodides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 3268-21-1

Figure 15 illustrates synthesis of tetracarboxylate ligand 4 in accordance with one embodiment. The synthesis of (3) shown in Figure 15 includes, in one embodiment, combining 1,4-diiodo-2,3,5,6-tetramethylbenzene (shown as (1) in Figure 15 and can be purchased from VWR) (0.60 g, 1.55 mmol) and 3,5-Bis(methoxycarbonyl) phenylboronic acid pinacol ester (shown as (2) in Figure 15 and prepared following Chen et al., A new multidentate hexacarboxylic acid for the construction of porous metal-organic frameworks of diverse structures and porosities, Cryst. Growth Des. 10, 2775-2779 (2010) (1.09 g, 3.41 mmol), K3PO4(1.97 g, 9.30 mmol) and dioxane (15 ml) in 10-20 ml capacity microwave vials and degassed for 10 min with nitrogen. Pd(PPh3)4(0.040 g, 0.03 mmol) was added and the vial was microwave heated with stirring at 150C for 6 hours. After cooling, CH2CI2(30 mL) was added and the organic layer was washed with water (20 raLchi3). The organic layer was dried over MgS04and evaporated under vacuum. The resulting solid was washed with MeOH and then dried under vacuum to give a white solid (0.S6 g, 70%). NMR (S00 MHz, CDCI3): 5 8.73 (t,J= 1.5Hz 2H), 8.10 (d, J = I.6Hz, 4H), 3.99 (s, 12H), 1.94 (s, 12H); 13C NMR (125MHz, CDCI3) delta 166.4, 143.4, 139.8, 134.8, 132.0, 130.9, 129.1, 52.5, 18.2.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3268-21-1, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NORTHWESTERN UNIVERSITY; WILMER, Christopher, E.; LEAF, Michael; SNURR, Randall, Q.; FARHA, Omar, K.; HUPP, Joseph, T.; WO2013/58844; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 148870-57-9, 148870-57-9

7,8-Dimethoxy-3-[3-iodopropyl]-l,3-dihydro-2H-3-benzazepin-2-one (38g) and potassium carbonate (6Og) were added to a mixture of (S)-N-[(4,5-dimethoxybenzocyclobut-l-yl)-methyl]- 7V-(methyl)amine (2Og) and demineralized water (100ml) at room temperature. The reaction mixture was heated and stirred at 50-55 C for 12-16 hours. After completion of reaction, reaction mass was cooled to 25-30 0C and the product is extracted in ethyl acetate (100ml). The aqueous layer was further extracted with ethyl acetate (60ml). Combined ethyl acetate layers was acidified with aqueous hydrochloric acid and stirred. The layers were separated and pH of the aqueous layer was adjusted to 10.5-12.5 with aqueous sodium hydroxide solution. The aqueous layer is extracted with ethyl acetate (140ml + 60ml). Ethyl acetate was distilled out completely under vacuum to get the title compound.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; IND-SWIFT LABORATORIES LIMITED; WO2008/146308; (2008); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 148870-57-9 as follows. 148870-57-9

Example 1:Preparation of 7,8-dimethoxy-3- [3- [[(1 S)-(4,5-dimethoxybenzocyclobutan-1- yl)methyl] methylamino] propyll-1 ,3-de-hydro-7,8-dimethoxy-2H-3-benzazepin-2-one oxalate (De-hydro ivabradine oxalate salt) 3-[3-lodopropylj-7,8-dimethoxy- I H-3-benzazepin-2(3H)-one (100 gm),dimethylformamide (800 ml), potassium carbonate (140 gm) and (S)-N-[(4,5-dimethoxybenzocyclobut- 1 -yl)-methyl]-N-(methyl)amine hydrochloride (40 gm) were added and then heated to 40 to 45C. The reaction mass was maintained for 17 hours at 40 to 45C and then cooled to room temperature. To the reaction mass were added hydrochloric acid (iN, 3000 ml) and ethyl acetate (2000 ml). The layers were separatedand the aqueous layer was extracted with ethyl acetate. Combined organic layers were dried with sodium sulfate and then concentrated to obtain a residual solid. To the residual solid was added ethyl acetate (750 ml) and then added a solution of oxalic acid (27 gm) in acetone (100 ml). The reaction mass was stirred for 2 hours at room temperature and filtered. The solid obtained was dried to obtain 90 gm of de-hydro ivabradine oxalate salt.Chromatographic purity of de-hydro ivabradine oxalate salt: 96.5%.

According to the analysis of related databases, 148870-57-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HETERO RESEARCH FOUNDATION; PARTHASARADHI REDDY, Bandi; RATHNAKAR REDDY, Kura; MURALIDHARA REDDY, Dasari; SRINIVASA RAO, Thungathurthy; VAMSI KRISHNA, Bandi; WO2013/150544; (2013); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

The chemical industry reduces the impact on the environment during synthesis 61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic acid, I believe this compound will play a more active role in future production and life. 61203-48-3

Examples 13.b.-16.b.[207] The intermediate 4-amino-6,7-methylenedioxyquinoline o-iodobenzamide derivatives used in Examples 13.a.-16.a. were prepared using the following general procedure. [208] A 2.0M solution of oxalyl chloride in CH2Cl2 (1.3 equiv.) was added to a solution of 2-iodo-5,6-dimethoxybenzoic acid (1.0 equiv.) in anhydrous CH2Cl2 (¡ì 60 mL per 10 mmol benzoic acid) and the solution stirred at reflux for 3 h. The mixture was allowed to cool and was then concentrated to dryness in vacuo. To the residue was added a solution of appropriate 4-amino-6,7-dimethoxyquinoline (1.0 equiv), triethylamine (2 equiv.) in CH2Cl2 (¡ì 60 mL per 4 mmol aminoquinoline). The reaction mixture was then stirred at reflux under N2. . In the case of those derivatives that have an alkylamine incorporated in their structure, the residue was partitioned between CHCl3 and 10% NaOH. The aqueous layer was repeatedly separated with CHCl3. All of the CHCl3 solutions (initial partition and extracts) were combined and dried (MgSO4). The aqueous layer was neutralized with 20% NaOH and extracted with CHCl3, dried (MgSO4) and evaporated. [209] Example 13.b. N-(6,7-Methylenedioxyquinolin-4-yl)-N-[(2-(t- butyldimethylsilanyloxy)-ethyl]-2-iodo-4,5-dimethoxybenzamide. Prepared from 4-[N-[2-(t-Butyldimethylsilanyloxy)]ethyl]amino-6,7-methylenedioxyquinoline (400 mg, 1.15 mmol) in 51.7% yield with a reaction time of 12 h, from the acid chloride prepared using 5.0 mmol of oxalyl chloride and 1.38 mmol of 2-iodo-5,6- dimethoxybenzoic acid. Compound 8h had: mp 79-80 qC; IR (KBr); 1653 1H NMR (CDCl3); 0.004 (d, 3H, J = 4.2Hz), 0.82 (s, 9H), 3.26 (s, 3H), 3.67 (s, 3H), 3.84- 4.02 (m, 4H), 6.13 (d, 2H, J = 4Hz), 6.40 (s, 1H), 7.02 (s, 1H), 7.33 (d, 1H, J = 4.2Hz), 7.36 (s, 1H), 7.42 (s, 1H), 8.52 (d, 1H, J = 4Hz); HRMS calcd for C27H33ISiN2O6H 637.1232; observed 637.1212

The chemical industry reduces the impact on the environment during synthesis 61203-48-3. I believe this compound will play a more active role in future production and life.

Reference:
Patent; GENZYME CORPORATION; TEICHER, Beverly A.; SCHMID, Steven M.; WO2012/15875; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

629-09-4, Adding a certain compound to certain chemical reactions, such as: 629-09-4, name is 1,6-Diiodohexane, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 629-09-4.

3,3′-(1,9-Decanediyn-1,10-diyl)-bis-pyridine (1 mmol) and an equivalent of 1,6-diiodohexane were mixed in acetonitrile (1000 mL). The mixture was refluxed for 7 days. The solvent was removed in vacuum after cooling and the resulting residue was taken up in water and partitioned between ethyl ether and water. The aqueous layer was extracted extensively with ethyl ether remove the starting materials. Most of the water was removed and the residue was transferred into methanol. Methanol was removed and the product was dried under vacuum to afford the bis-pyridinium cyclophane (30% yield). HNMR (300 MHz, D2O) 8.76 (s, 2H), 8.56 (d, J=6.0 Hz, 2H), 8.29 (d, J=8.4 Hz, 2H), 7.81 (dd, J=6.3 Hz, 8.1 Hz, 2H), 4.40 (t, J=7.5 Hz, 4H), 2.39 (t, J=6.3 Hz, 4H), 1.85-1.84 (m, 4H), 1.49-1.52 (m, 4H), 1.38-1.42 (m, 4H), 1.18-1.22 (m, 4H). CNMR, 146.97, 146.26, 142.61, 128.00, 125.71, 101.43, 73.93, 61.99, 29.94, 27.84, 27.49, 24.43, 18.90.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1,6-Diiodohexane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; UNIVERSITY OF KENTUCKY RESEARCH FOUNDATION; US2010/222377; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 3268-21-1 as follows. 3268-21-1

A 200 mL four-neck flask equipped with a stirrer was charged with zinc chloride (7.00 g, 51.4 mmol) and tetrahydrofuran (70 mL) under nitrogen atmosphere, and with stirring, 1,1,1,2-tetrafluoroethane (7.70 g, 75.5 mmol) was blown thereinto at -20 C. Next, a tetrahydrofuran-n-hexane solution of lithium diisopropylamide (1.1 M, 99 mL, 108.5 mmol) was gradually added thereto with the dropping port dipped in the liquid content, and the mixture was stirred at room temperature for 30 minutes. Subsequently, 1,4-diiodo-2,3,5,6-tetramethylbenzene (5.41 g, 14.0 mmol) and tetrakis(triphenylphosphine)palladium (0.65 g, 0.6 mmol) were introduced thereinto and the mixture was stirred at 50 C. for 48 hours. After cooling, an aqueous hydrochloric acid solution was added thereto and the organic layer was washed with 20% saline (50 mL*3 times). The resulting organic layer was dried over anhydrous magnesium sulfate and then the filtrate was concentrated under reduced pressure. The concentrate obtained was purified by silica gel chromatography to give 3.18 g of white solid 1,4-bis(trifluorovinyl)-2,3,5,6-tetramethylbenzene (purity=95.7 wt %, isolated yield=74%). (Results of Analysis) 1H-NMR (Acetone-d6, 400 MHz); 2.18 ppm (d, 12H, Me). 19F-NMR (Acetone-d6, 376 MHz); -158.9 ppm (dd, 2F), -118.3 ppm (ddd, 2F), -104.8 ppm (ddd, 2F). m.p. 91-94 C. GC-MS (m/z):294 (m, 60), 279 (15), 259 (5), 243 (100), 228 (9), 177 (15), 159 (9), 133 (6), 51 (8).

According to the analysis of related databases, 3268-21-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TOSOH FINECHEM CORPORATION; MIYAUCHI, Hideki; KONDO, Norihisa; NAGASAKI, Noritaka; US2020/17429; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

615-42-9, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 615-42-9, name is 1,2-Diiodobenzene, A new synthetic method of this compound is introduced below.

[00150] Copper (I) iodide (FW 190.45, 0.90 grams, 4.72 mmol), 1,10-phenanthroline (FW 180.21, 0.83 grams, 4.62 mmol), cesium carbonate (FW 325.82, 19.00 grams, 58.30 mmol), 1 ,2-diiodobenzene (FW 329.90, 7.50 grams, 22.70 mol), di(ethylene glycol) ethyl ether (FW 134.17, 9.18 grams, 68.40 mol) and 100 milliliters of dry xylene were charged in a 350 milliliter three necked round bottom flask. The reaction mixture was heated with stirring at reflux temperature for 20 hours under nitrogen. The resulting suspension was cooled to room temperature by adding 50 milliliters of toluene. Then reaction mixture was filtered through celite and alumina. The low boiling (xylene and toluene) component was removed by a rotary evaporator and high boiling component di(ethylene glycol) ethyl ether by air bath oven at 200C under high vacuum for 2 hours. The residue was purified by flask chromatography on silica gel. The final dark yellow product yielded 7.00 grams (90%). The product I and C NMR analysis shows the formation of aryl ether product. IR: neat (cm” FontWeight=”Bold” FontSize=”10″ ): 745, 843, 931, 1052, 1 1 16, 1219, 1256, 1325, 1350, 1373, 1453, 1501, 1593, 2869, 2929, 2973. 1H NMR (CDC13): delta 6.76 (m, 4H, Ph), 4.02 (t, 4H, -OCH2-), 3.71 (m, 4H, -CH2O-) 3.57 (m, 4H, -OCH2), 3.45(m, 4H, -OCH2-), 3.37(t, 4H, -OCH2-), 1.06 (t, 6H, -CH3). 13C NMR (CDC13): 149.42, 121.61, 1 15.04, 70.89, 69.89, 69.76, 68.93, 66.59, 15.14.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; EXXONMOBIL RESEARCH AND ENGINEERING COMPANY; PATIL, Abhimanyu, Onkar; BODIGE, Satish; WO2015/60985; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

61203-48-3, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 61203-48-3, name is 2-Iodo-4,5-dimethoxybenzoic acid, This compound has unique chemical properties. The synthetic route is as follows.

[230] b. N-(6,7-Methylenedioxyquinolin-4-yl)-N-[2-(N,N-diethylamino)ethyl]-2- iodo-4,5-dimethoxybenzamide. Oxalyl chloride (1.12 g , 8.8 mmol) was added to a solution of 2-Iodo-4,5-dimethoxybenzoic acid (820 mg, 2.6 mmol; see above) in anhydrous methylene chloride (40 mL) and the stirred mixture was refluxed for 4 hours. The mixture was then concentrated to dryness under reduced pressure. The acid chloride was dissolved in 40 mL of methylene chloride and added to a solution of 4-[[2-(Diethylamino)ethyl]amino]-6,7-methylenedioxyquinoline (640 mg, 2.2 mmol), and triethylamine (2.2g, 22 mmol) in methylene chloride (50 mL) and the resulting mixture was stirred at reflux under nitrogen for 2 hours. The reaction mix was cooled and washed with a saturated solution of sodium bicarbonate (3 x 75 mL), and extracted into dilute HCl (4 x 100 mL). The aqueous extract was then neutralized with 30% NaOH and extracted with CHCl3 (4 x 100 mL), washed with brine (100mL), dried (MgSO4) and evaporated, yielding 1.1 g as a sticky semisolid glue, in 86% yield; 1H NMR (CDCl3) 0.96 (t, 6H, J=7.2), 2.54 (q, 4H, J=7.2), 2.82 (m, 2H), 3.29 (s, 3H), 3.71 (s, 3H), 3.92 (m, 1H), 4.46 (m, 1H), 6.12 (s, 2H), 6.37 (s, 1H), 7.00 (s, 1H), 7.27 (d, 1H, J=4.8), 7.33 (s, 1H), 7.39 (s, 1H), 8.52 (d, 1H, J=4.8); 13C NMR (CDCl3) 11.8, 47.1, 47.5, 50.7, 55.5, 56.1, 82.7, 98.5, 102.2, 106.7, 110.6, 120.1, 121.8, 122.7, 133.7, 146.3, 148.1, 148.3, 148.5, 149.0, 149.7, 151.0, 170.0; HRMS calcd for C25H28O5N31H: 578.1153; found: 578.1153.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; GENZYME CORPORATION; TEICHER, Beverly A.; SCHMID, Steven M.; WO2012/15875; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com