Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 624-76-0, name is 2-Iodoethanol, 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 624-76-0, category: iodides-buliding-blocks

To the mixture of 4-iodopyridin-2(1H)-one (50 mg, 0.213 mmol) in DMF (3 mL) was added 2-iodoethanol (73 mg, 0.426 mmol), K2CO3 (88 mg, 0.638 mmol) at rt. The mixture was stirred for 2 h at rt. After the reaction was finished, the mixture was washed with water and extracted with EtOAc. The organic phase was washed with brine, dried over Na2SO4, filtered, and concentrated to give the crude product, which was purified by TLC to provide 1-(2-hydroxyethyl)-4-iodopyridin-2(1H)-one (60 mg 100%).

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, 2-Iodoethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Vitae Pharmaceuticals, Inc.; Boehringer Ingelheim International GmbH; US2010/331320; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 624-76-0,Some common heterocyclic compound, 624-76-0, name is 2-Iodoethanol, molecular formula is C2H5IO, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

taking theobromine 540mg (3mmoL), NaH 720mg (30mmol) dissolved in 80mL DMF, adding 2mmol of 2-iodoethanol under the drop, after 4 hours of reaction, quenching the reaction with water, spin dry, oil Ether: CH3CH2OCOCH3 = 3:1 (v/v) as a mobile phase over silica gel to give compound 1-ethylhydroxy-3-7-dimethylxanthine, yield 94%.

The synthetic route of 624-76-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan University Huaxi Hospital; Huang Wen; (18 pag.)CN109912598; (2019); A;,
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 624-75-9 as follows. Recommanded Product: 2-Iodoacetonitrile

To a solution of 5-chloro-2-isopropyl-4-methoxy-phenol (10.36 g, 51.6 mmol) in 40 mL DMF was added K2CO3 (8.55 g, 62.0 mmol) and the mixture was heated to 65 C. After 15 minutes iodoacetonitrile (9.05 g, 54.2 mmol) was added and the mixture was heated to 80 C. for 1 hour. The mixture was cooled, poured into an ice/H2O mixture and extracted with 1:1 toluene/hexane. The combined organics were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by passing through a short plug of silica to afford (5-chloro-2-isopropyl-4-methoxy-phenoxy)-acetonitrile (11.97 g, 97%) as a white solid.

According to the analysis of related databases, 624-75-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Roche Palo Alto LLC; US2007/49609; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 624-75-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 624-75-9, name is 2-Iodoacetonitrile belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Add 0.95 Kg of iodoacetonitrile and 500 g of anhydrous calcium fluoride to a 3-liter reaction flask at room temperature, add 600 ml of 3-pentanone, turn on the electric stirrer and start Heating, the temperature rose to 100 C, reaction 2.5h.2. After the above reaction, cool to 52 C, install the distillation unit, raise the temperature to 110 C, distillation, and the liquid bottle is cooled with dry ice until no liquid flows out. The product yield was 95.7% and the purity reached 96.6%.3. The above product was placed in a 500 ml single-necked flask and distilled at 120 C under normal pressure to collect 78-80 C fractions. The vial was cooled with an acetone bath to give a mixture of fluoroacetonitrile having a purity of 99.8%

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, 2-Iodoacetonitrile, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BSAZ BIOTECH (HANGZHOU) CO.LTD.; Wang, zheming; Yang, yewei; Jiang, shikun; (5 pag.)CN104230753; (2016); B;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 7681-82-5, name is Sodium iodide, A new synthetic method of this compound is introduced below., Application In Synthesis of Sodium iodide

General procedure: A typical example is exemplified by the synthesis of 4b: To a stirred solution of TMEDA (1.36 mL,9 mmol) in hexane (5 mL) was added dropwise at ice bath temperature n-butyllithium (9 mmol) in hexane followed by acetophenone trimethylsilyl enol ether 1 (576 mg, 3 mmol), and the mixture was stirred for 24 h at room temperature. In a separate flask, a mixture of bismuth(III) chloride (315.5 mg,1 mmol) and tris(4-methylphenyl)bismuthane (964 mg, 2 mmol) was stirred in ether (10 mL) at room temperature for 1 h. To the suspension of chlorobis(4-methylphenyl)bismuthane (ca. 3 mmol) thus formed was added sodium iodide (450 mg, 3 mmol) and a few drops of 15-crown-5 ether and the resulting yellowish mixture was stirred for 3 h at room temperature. To a suspension of the lithium compound previously prepared was added at room temperature magnesium dibromide diethyl etherate (775 mg, 3 mmol) followed by, at -30 C, a suspension of iodobis(4-methylphenyl)bismuthane(ca. 9 mmol), and the resulting mixture was stirred for 1 h, during which time the temperature was raised to ambient temperature. The reaction mixture was poured into brine (50 mL) and extracted with ethyl acetate (50 mL ¡Á 3). The combined extracts were concentrated to leave an oily residue, which was purified by chromatography (silica gel) using hexane-ethyl acetate (5:1) as the eluent to afford 4b in 30% yield (459 mg, 0.9 mmol). Because 4a, 4f and 10 underwent decomposition when purified by chromatography on silica gel, these compounds were converted into the corresponding halobismuthanes 5a, 5f and 11, respectively, without isolation.

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:
Article; Murafuji, Toshihiro; Tomura, Mai; Ishiguro, Katsuya; Miyakawa, Isamu; Molecules; vol. 19; 8; (2014); p. 11077 – 11095;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 7681-82-5, name is Sodium iodide, 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 7681-82-5, Computed Properties of INa

To a dry round-bottom flask with a stir bar was added 5c (245 mg, 0.983 mmol) and NaI (460 mg, 3.06 mmol). Chlorotrimethylsilane (375 muL, 2.95 mmol) was added dropwise over 5 min at 0C, allowed to stir at 0C for 5 more min, and warmed to rt for 3 hr. The mixture was concentrated, dissolved in ether (25 mL) and 1M HCl (~10 mL), and transferred to a separatory funnel. The aqueous layer was extracted once more with ether (25 mL) and combined organics were washed once with with sat?d NaHSO3 and once with sat?d brine. The organic layer was dried over Na2SO4, filtered, concentrated, and dried in vacuo to afford a dry, white solid 7 (181 mg, 72%) which did not require further purification .1H NMR (CDCl3, 400 MHz) delta 4.52 (s, 2H), 5.06 (s, 2H), 7.29 (d, 1H, J=7.9), 7.51 (d, 1H, J=7.8), 7.75 (s, 1H).13C NMR (CDCl3, 100 MHz) delta 5.47, 71.21, 121.66, 130.50, 131.77, 138.51, 153.53. 11B NMR (CDCl3, 128 MHz) delta 32.24. HRMS (MAII) calc. for C8H8BO2 [M-I]+ 147.0612, found 147.0623.

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, Sodium iodide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; UNIVERSITY OF THE SCIENCES; TOMSHO, John, W.; GAMRAT, James, M.; (0 pag.)WO2019/173814; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 7681-82-5, name is Sodium iodide, 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 7681-82-5, Recommanded Product: Sodium iodide

Complex [Pd(P,P)Cl2] (0.070?g, 0.113?mmol) was dissolved at room temperature in aceton (10?mL), followed by the addition of NaI in stoichiometric excess (0.070?g, 0.452?mmol), affording a dark yellow solution, which was stirred at room temperature for 24?h. The reaction mixture was then concentrated to dryness and the solid residue was re-dissolved in dichloromethane (10?mL). This solution was filtrated through celite in order to remove the remaining NaI or NaCl formed during the reaction. The filtrate was concentrated to 4?mL, n-hexane (10?mL) were then added to allow precipitation of the expected product, that was collected by filtration, and dried under vacuum to afford 0.060?g (67% yield) of a dark yellow powder, m.p. (dec.)?>?200?C. IR (KBr, cm-1): 506 (s), 528 (m), 562 (s), 591 (m), 692 (s), 748 (s), 867 (s) nu(P-N-P), 995 (m), 1101 (s), 1097 (s), 1176 (s), 1224 (s), 1245 (s), 1307 (w), 1375 (m), 1434 (s) nu(P-Ph), 1457 (s), 1480 (s). 1H NMR (600?MHz, CDCl3): delta 8.23 (m, 8H, Ar), 7.68-7.65 (m, 4H, Ar), 7.61-7.59 (m, 8H, Ar), 0.96 (s, 9H, tBu). 31P{1H} NMR (121.5?MHz, CDCl3): delta 25.09. HRMS (positive ESI-MS): calcd for C28H29INP2Pd [M?-?I]+ 673.9849, found 673.9877; calcd for C28H29I2NNaP2Pd [M+Na]+ 823.8792, found 823.8830.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Sodium iodide, and friends who are interested can also refer to it.

Reference:
Article; Ioannou, Polydoros-Chrysovalantis; Arbez-Gindre, Cecile; Zoumpanioti, Maria; Raptopoulou, Catherine P.; Psycharis, Vassilis; Kostas, Ioannis D.; Kyritsis, Panayotis; Journal of Organometallic Chemistry; vol. 879; (2019); p. 40 – 46;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

The chemical industry reduces the impact on the environment during synthesis 624-75-9, name is 2-Iodoacetonitrile, I believe this compound will play a more active role in future production and life. 624-75-9

e) To a solution of 7-benzyloxymethyl-8-(4-hydroxyphenyl)-1,3-dipropyl-1,3,7-trihydropurine-2,6-dione (1 g, 2.2 mmol) in tetrahydrofuran (20 ml) was added potassium t-butoxide (0.28 g, 2.4 mmol), and the mixture stirred for 30 minutes at room temperature. Iodoacetonitrile (0.38 g, 2.23 mmol) was then added, and the mixture stirred for 16 hours at room temperature. The solvent was removed under reduced pressure, and the residue was dissolved in ethyl acetate and passed through a silica gel plug, to provide 7-benzyloxymethyl-8-(4-cyanomethoxyphenyl)-1,3-dipropyl-1,3,7-trihydropurine-2,6-dione, a compound of formula (7)

The chemical industry reduces the impact on the environment during synthesis 624-75-9. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Kalla, Rao; Perry, Thao; Elzein, Elfatih; Varkhedkar, Vaibhav; Li, Xiaofen; Ibrahim, Prabha; Palle, Venkata; Xiao, Dengming; Zablocki, Jeff; US2005/261316; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

624-75-9, 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 624-75-9 as follows.

The compound obtained in Example 21 (4.6 g, 15.35 mmol) and potassium carbonate (10.6 g, 76.73 mmol) were added to acetone (100 mL) and refluxed for 2 hours by heating. To this reaction mixture was dropwise added iodoacetonitrile (1.34 mL, 18.42 mmol), and refluxed over 2 hours. The acetone was removed by vacuum distillation, and to the residue were added water (200 mL) and ethyl acetate (200 mL). The organic layer was dried over anhydrous magnesium sulfate and distillated in a vacuum. The concentrate was subjected to column chromatography (silica gel, ethyl acetate-hexane 2:3 v/v) to afford a mixture of 2:1 of [4-(2-chloropyridin-4-yl)-3-(3-methoxy-5-methylphenyl)-1H-pyrazol-1-yl]acetonitrile and [4-(2-chloropyridin-4-yl)-5-(3-methoxy-5-methylphenyl)-1H-pyrazol-1-yl]acetonitrile as yellow oil. These two regioisomers (4.78 g, 92%) were used in the next reaction step without separation.[4-(2-Chloropyridin-4-yl)-3-(3-methoxy-5-methylphenyl)-1H-pyrazol-1-yl]acetonitrile: 1H NMR (CDCl3) delta 2.29 (s, 3H), 3.71 (s, 3H), 5.19 (s, 2H), 6.73 (s, 1H), 6.75 (s, 1H), 6.85 (s, 1H), 7.06 (d, J=4.4 Hz, 1H), 7.26 (s, 1H), 7.79 (s, 1H), 8.24 (d, J=4.8 Hz, 1H); 13C NMR (CDCl3) delta 21.53, 39.97, 55.29, 110.91, 111.12, 113.65, 115.67, 118.75, 121.59, 121.65, 122.78, 130.58, 132.37, 140.16, 143.28, 149.68, 151.45, 151.79, 159.71, 162.33.[4-(2-Chloropyridin-4-yl)-5-(3-methoxy-5-methylphenyl)-1H-pyrazol-1-yl]acetonitrile: 1H NMR (CDCl3) delta 2.39 (s, 3H), 3.83 (s, 3H), 4.94 (s, 2H), 6.63 (s, 1H), 6.74 (s, 1H), 6.92-6.96 (m, 2H), 7.19 (s, 1H), 7.93 (s, 1H), 8.17 (d, J=5.2 Hz, 1H); 13C NMR (CDCl3) delta 21.56, 37.78, 55.48, 112.15, 113.91, 117.08, 118.16, 119.88, 121.36, 122.48, 128.46, 139.57, 141.60, 142.19, 142.85, 149.78, 151.95, 160.48.To a solvent mixture of THF and water (4:1, 10 mL) were added the mixture prepared in Example 22 (320 mg, 0.95 mmol), 4-acetylphenyl boronic acid (0.19 g, 1.13 mmol), dichlorobis(triphenylphosphine)palladium (II) (33 mg, 0.05 mmol) and potassium carbonate (131 mg, 0.95 mmol), and stirred at 70 C. for 12 hours under nitrogen atmosphere. The reaction mixture was cooled at room temperature, washed with ice water (100 mL) and extracted with ethyl acetate (100 mL¡Á3). The organic extract was dried over anhydrous magnesium sulfate and distilled under vacuum. The residue was subjected to prep-TLC using a solvent mixture of ethyl acetate/hexane to purify the desired products.Purification yield by prep-TLC (silica gel, ethyl acetate-hexane, 1:2, v/v): (93 mg, 75%); m.p. 156-157 C.; 1H NMR (CDCl3) delta 2.42 (s, 3H), 2.65 (s, 3H), 3.82 (s, 3H), 4.97 (s, 2H), 6.75 (s, 1H), 6.82 (s, 1H), 6.96 (s, 1H), 7.12 (d, J=4.9 Hz, 1H), 7.60 (s, 1H), 7.87 (d, J=8.1 Hz, 2H), 7.99-8.02 (m, 3H), 8.56 (d, J=5.1 Hz, 1H); 13C NMR (CDCl3) delta 21.60, 26.78, 37.78, 55.52, 112.34, 114.02, 116.86, 118.62, 119.33, 120.38, 122.67, 126.90, 128.76, 129.01, 137.12, 139.56, 140.61, 141.58, 141.96, 143.49, 150.20, 156.29, 160.54, 197.88.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 624-75-9, and friends who are interested can also refer to it.

Reference:
Patent; LEE, So Ha; Yoo, Kyung Ho; Oh, Chang Hyun; Han, Dong Keun; El-Deeb, Ibrahim Mustafa; Park, Byung Sun; Jung, Su Jin; US2011/15395; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

627-32-7,Some common heterocyclic compound, 627-32-7, name is 3-Iodo-1-propanol, molecular formula is C3H7IO, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Cesium carbonate [(5.] 54 g) is added to a solution [OFN (4-CHLOROBENZYL)-4-HYDROXY 2-] (hydroxymethyl) thieno [2, [3-B]] [PYRIDINE-5-CARBOXAMIDE] (5.23 g, prepared as described in US 6,239, 142) and 2-(3-iodopropoxy)tetrahydro-2H-pyran (4.32 g, prepared by mixing equal molar amounts of 2-iodopropanol and 3, 4-dihydro-2H-pyran) in DMF (20 mL). The mixture is heated at [60 C] for 4 hours. The solvent is evaporated and the residue is dissolved in 10% [MEOH] in [CH2C12.] The mixture is washed with water and the organic layer is dried (MgSO4), filtered, and concentrated. The crude product is purified by column chromatography [(CH2CLJMETHANOL,] [95/5)] followed by recrystallization from EtOAc to afford 4.82 g of the title compound as white crystals. Physical characteristics. 1H NMR (400 [MHZ,] DMSO-d6) 8 10.55, 8.71, 7.39, 7.33, 7.29, 5.79, 4. [70,] 4.53, 4.49, 4. [38, 3.] 68,3. [37,] 2.11, 1.63, 1.53, 1.40 ; MS [(EI)] m/z 490 [(MF)] ; Anal. Found: C, 58.74 ; H, 5.66 ; N, 5.61.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Iodo-1-propanol, its application will become more common.

Reference:
Patent; PHARMACIA & UPJOHN COMPANY; FLECK, Bruce, Francis; WO2004/22567; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com