Month: February 2021

Application 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.

The compound obtained in Example 64 (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. 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 the residue was treated in 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 regioisomers as yellow oil. These two regioisomers (4.16 g, 80%) were used in the next reaction step without separation.Example 65-2Preparation of 4-(2-chloropyridin-5-yl)-5-(3-methoxy-5-methylphenyl)-pyrazol-1-yl)acetonitrile1H NMR (CDCl3) delta 2.28 (s, 3H), 3.66 (s, 3H), 5.16 (s, 2H), 6.71 (s, 2H), 6.84 (s, 1H), 7.24 (d, J=8.3 Hz, 1H), 7.49 (dd, J=2.3, 5.9 Hz, 1H), 7.70 (s, 1H, 8.32 (s, 1H); 13C NMR (CDCl3) delta 21.57, 39.89, 55.23, 110.80, 113.76, 115.28, 117.76, 121.47, 124.02, 127.24, 129.92, 132.57, 138.58, 140.12, 148.71, 149.92, 151.17, 159.69, 162.33.To a solvent mixture of THF and water (4:1, 10 mL) were added the mixture prepared in Example 65 (0.3 g, 0.89 mmol), 2-acetylphenylboronic acid (0.18 g, 1.07 mmol), dichlorobis(triphenylphosphine)palladium (II) (32 mg, 0.05 mmol) and potassium carbonate(0.13 g, 0.89 mmol). The reaction system was purged with nitrogen gas for 10 min, and stirred at 70 C. for 12 hours under nitrogen atmosphere. The reaction mixture was cooled to 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): (72 mg); m.p. 72-73 C.; 1H NMR (CDCl3) delta 2.18 (s, 3H), 2.36 (s, 3H), 3.78 (s, 3H), 4.95 (s, 2H), 6.68 (s, 1H), 6.75 (s, 1H), 6.86 (s, 1H), 7.43-7.59 (m, 6H), 7.91 (s, 1H), 8.49 (s, 1H); 13C NMR (CDCl3) delta 21.55, 30.49, 37.81, 55.38, 112.37, 114.78, 116.72, 118.33, 122.13, 122.67, 126.78, 127.62, 128.64, 128.92, 128.99, 130.26, 134.89, 138.22, 139.49, 141.23, 141.33, 141.58, 147.50, 155.33, 160.40, 204.23.

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; 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

Application of 42861-71-2, The chemical industry reduces the impact on the environment during synthesis 42861-71-2, name is 3-Iodophenyl acetate, I believe this compound will play a more active role in future production and life.

Intermediate- 17: 3-(Trimethylsilanylethynyl)-phenylacetate; To a solution of 3-acetoxy iodobenzene (6.0 g, 22.89 mmoles) in DMSO (25 mL) was added trimethylsilyl acetylene (1.1 eq) followed by triethylamine (3 eq), CuI (0.05 eq) and tetrakis (triphenylphosphine) palladium(O) (0.03 eq) and the reaction’ mixture was stirred at room temperature for 6 h. The reaction mixture was then diluted with water and extracted with ethyl acetate. The organic layer was then dried over Na2SO4, concentrated and purified by column chromatography to get 4.3 g of the desired product. 1H NMR (CDCl3) delta 7.30-7.25 (m, 2H), 7.18 (s, IH), 7.05-6.95 (m, IH), 2.28 (s, 3H), 0.24 (s, 9H).

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, 3-Iodophenyl acetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GLENMARK PHARMACEUTICALS S.A.; GHARAT, Laxmikant, Atmaram; NARAYANA, Lakshminarayana; THOMAS, Abraham; KHAIRATKAR-JOSHI, Neelima; SHAH, Daisy, Manish; WO2010/7482; (2010); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 103962-05-6, The chemical industry reduces the impact on the environment during synthesis 103962-05-6, name is 1-Iodo-4-(trifluoromethoxy)benzene, I believe this compound will play a more active role in future production and life.

CuI (0.26 g, 1.378 mmol), 2-picolinic acid (0.24 g, 1.969 mmol), and cesium carbonate (19.24 g, 59.061 mmol) were combined, evacuated and filled with argon (3 times). 1,4-Dioxane was then added followed by diethylmalonate (6 mL, 39.374 mmol) and 1-iodo-4-(trifluoromethoxy)benzene (3 mL, 19.687 mmol). The resulting yellow suspension was stirred at room temperature for 48 hours and quenched with saturated NH4Cl. The mixture was extracted with EtOAc (2¡Á). The combined organic extracts were dried over Na2SO4, filtered, and concentrated to provide 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, 1-Iodo-4-(trifluoromethoxy)benzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Janssen Pharmaceutica NV; Leonard, Kristi A.; Barbay, Kent; Edwards, James P.; Kreutter, Kevin D.; Kummer, David A.; Maharoof, Umar; Nishimura, Rachel; Urbanski, Maud; Venkatesan, Hariharan; Wang, Aihua; Wolin, Ronald L.; Woods, Craig R.; Fourie, Anne; Xue, Xiaohua; Mirzadegan, Taraneh; Ganamet, Kelly; US2014/107097; (2014); A1;,
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. 19099-54-8, name is 1-Iodo-2-isopropylbenzene, A new synthetic method of this compound is introduced below., Quality Control of 1-Iodo-2-isopropylbenzene

General procedure: To a mixture of the catalyst 3 (20mg containing 0.05mol% Pd for aryl iodides and 40mg containing 0.1mol% Pd for aryl bromides and chlorides), aryl halide (1mmol), alkyne (1.5mmol), and K2CO3 (1.5mmol, 207mg) was added PEG 200 (2mL) under argon atmosphere. The reaction mixture was stirred for the appropriate reaction time at 85 or 130C (see, Table 2). The progress of the reaction was monitored by using gas chromatography. After completion of the reaction, pure products were obtained by using column chromatography with hexane and ethyl acetate as eluents.

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; Gholinejad, Mohammad; Dasvarz, Neda; Najera, Carmen; Inorganica Chimica Acta; vol. 483; (2018); p. 262 – 270;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 628-21-7, name is 1,4-Diiodobutane belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 628-21-7

Preparation 122 4′-Chlorospiro[cyclopentane-1,5′-pyrrolo[2,3-d]pyrimidin]-6′(7’H)-one Add 4-chloro-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one (0.6 g; 0.0035 mol; 1.0 equiv) in anhydrous THF (20 mL) and cool the reaction to -78 C., under an inert atmosphere. Add drop-wise lithium hexamethyldisilazide (8.8 mL; 0.0088 mol; 2.5 equiv; 1M in THF). Stir at -78 C. for 30 min. Add drop-wise 1,4-diiodobutane (0.56 mL; 0.0042 mol; 1.2 equiv), allow the reaction temperature to reach 0 C. slowly, and stir for 2 h. Then allow the reaction to reach RT and stir for additional 1 h. Quench the reaction with saturated ammonium chloride solution and extract with EA. Wash the organic layer with water, brine, and dry over anhydrous sodium sulfate. Evaporate the organic layer and purify over a 10 g silica column with acetone (5%) in DCM. Pool fractions to give the title compound (0.34 g; 43.09%). H NMR (DMSO-d6):11.68 (1H, s), 8.53 (1H, s), 2.0-2.1 (m, 2H), 1.91-1.99 (m, 6H).

The synthetic route of 628-21-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shepherd, Timothy Alan; Dally, Robert Dean; Joseph, Sajan; US2010/120801; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 13421-13-1

General procedure: To an oven dried three neck RB containing 2-Iodobenzoic acid (1) (2mmol), benzyl amine (2) (4mmol) and CuI(0.4mmol) in DMSO(3ml) was added 0.55g of K2CO3. Then, the reaction mixture was allowed to stir at 90C under air atmosphere for 12h.The completion of the reaction was monitored by TLC. After being cooled at room temperature the reaction mixture was poured in to ice cooled water and extracted with ethyl acetate two times. The combined organic layer was washed with brine and then dried over anhydrous Na2SO4. The solvent was evaporated and the crude product was purified by column chromatography (hexane(80)/ ethyl acetate (20)) on silica gel to afford 2-phenyl-4H-benzo[d][1,3]oxazine-4-one.

According to the analysis of related databases, 13421-13-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Munusamy, Sathishkumar; Venkatesan, Sathesh; Sathiyanarayanan, Kulathu Iyer; Tetrahedron Letters; vol. 56; 1; (2015); p. 203 – 205;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Reference of 3210-08-0, 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. 3210-08-0, name is 4-Iodobutan-1-ol belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Method B: Compound 3(68.9 mg, 0.074 mmol) was allowed to stir overnight in THF(10 mL) at 55 C. The solvent was removed from the product toafford pure 4 as a pale orange solid (65 mg, 87% yield). Yellow crystalssuitable for X-ray crystallography were grown from a concentratedCH2Cl2 solution of compound 4. 1H NMR (400 MHz, CD2Cl2):d 7.74 (m, 4H, Ar-H), 7.59 (m, 2H, Ar-H), 7.46 (m, 2H, Ar-H), 7.41(m, 8H, Ar-H), 7.27 (m, 2H, Ar-H), 7.18 (m, 2H, Ar-H), 7.07 (m,8H, Ar-H), 4.01 (m, 2H, O-CH2CH2CH2CH2-I), 3.88 (br, 2H, CH2),2.96 (m, 2H, O-CH2CH2CH2CH2-I), 2.54 (br, 2H, CH2), 1.67 (m, 2H,O-CH2CH2CH2CH2-I), 1.39 (m, 2H, O-CH2CH2CH2CH2-I). 31P NMR(161.8 MHz, CD2Cl2): d 93.1 (br, 1P), 10.7 (br, 2P). 13C NMR(100.5 MHz, C6D6): d 147.0, 135.6, 135.3, 134.1, 131.5, 130.0,129.6, 128.6, 124.3, 123.5, 66.8, 47.6, 33.2, 30.3, 7.0. Anal. Calc.for C42H40N2OP3CuI2: C, 50.49; H, 4.04; N, 2.80. Found: C, 50.22;H, 3.99; N, 2.77%.

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, 4-Iodobutan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Knight, Sadie E.; Bezpalko, Mark W.; Foxman, Bruce M.; Thomas, Christine M.; Inorganica Chimica Acta; vol. 422; (2014); p. 181 – 187;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 124700-41-0,Some common heterocyclic compound, 124700-41-0, name is 2-Fluoro-5-iodobenzoic acid, molecular formula is C7H4FIO2, 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.

Compound 1 (20.0 g, 75.2 mmol, 1 eq) was dissolved in 70 mL of EtOH.Then gradually add H2SO4 (7.37g, 75.1mmol, 4.01mL, 1eq).The mixture was stirred at 100 C for 5 h.And use TLC (Dichloromethane/Methanol=10/1, Rf=0.87) The progress of the reaction was detected.When the reaction is complete,The reactants were concentrated under reduced pressure.The concentrated product was extracted (EOtOH 200 mL, NaHCO 3 saturated solution (100.0 mL x 2), and then the organic layer was taken.It was dried by adding anhydrous Na2SO4.After further evaporation to dryness the title product 2 (21.0 g, 71.4 mmol, 94.9% yield).Figure 3 shows the results of TLC chromatography for this reaction.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Fluoro-5-iodobenzoic acid, its application will become more common.

Reference:
Patent; Shanghai Health Medical School; Tang Dewei; Huang Gang; Huang Chen; Wu Xingyu; Yu Meicen; Li Yanjiao; (18 pag.)CN109942582; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 608-28-6, These common heterocyclic compound, 608-28-6, name is 2-Iodo-1,3-dimethylbenzene, its 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.

Add 0.2 mmol of potassium carbonate,0.005 mmol of tris (dibenzylideneacetone) dipalladium,1,3-bis (diphenylphosphine) propane 0.02mmol,18-crown-6-ether 0.1mmol,1,3-dimethyl-2-iodobenzene 0.1 mmol,1-phenyl-1-hexyne 0.25 mmol and1 mL of N, N-dimethylformamide was added to a 15 mL reaction tube,Fill with nitrogen repeatedly 10 times, stir at room temperature for 15 min, add 0.5 mmol of water, and place in a reaction dish at 100 C for 16 h; cool to room temperature, dilute the reaction solution with ethyl acetate, wash with water, and dry the organic phase with anhydrous Na2SO4 , Filtered, concentrated, and purified by thin layer chromatography to obtain 14.9 mg of the target product as a colorless oil with a yield of 57%.

Statistics shows that 2-Iodo-1,3-dimethylbenzene is playing an increasingly important role. we look forward to future research findings about 608-28-6.

Reference:
Patent; Huaqiao University; Cheng Guolin; Lv Weiwei; (12 pag.)CN110256184; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 34270-90-1

A stirred solution of Intermediate 71 (0.8 g, 2.42 mmol) and 1-iodo-2-(2-iodoethoxy)ethane (0.38 mL, 2.67 mmol) in anhydrous DMF (16 mL) was cooled to -l5C30 and purged with nitrogen for 5 minutes, then caesium carbonate (3.16 g, 9.69 mmol) wasadded. The reaction mixture was stirred for 2 h, with warming to 20C. Water (30 mL)was added and the aqueous layer was extracted with tert-buty1 methyl ether (3 x 30 mL).The combined organic layers were washed with water (2 x 30 mL) and brine (30 mL), then dried over sodium sulfate, filtered and concentrated. The resulting crude materialwas purified by flash column chromatography, using a gradient of tert-buty1 methyl etherin heptane (0-15%), to afford the title compound (927.9 mg, 86%) as a yellow solid. DH(500 MHz, CDCb) 7.90 (d, J 1.3 Hz, 1H), 7.06 (dd, J9.1, 1.6 Hz, 1H), 4.26 (t, J 11.8 Hz,5 2H), 3.89 (dd, J 11.9, 3.6 Hz, 2H), 2.45-2.33 (m, 2H), 1.75-1.69 (m, 2H), 1.65 (s, 9H).HPLC-MS (method 5): [M+H-BOC]+ m/z 300.0, 302.0, RT 2.11 minutes.

According to the analysis of related databases, 34270-90-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UCB BIOPHARMA SPRL; BRACE, Gareth Neil; CHAPPELL, Rose Elizabeth; DEBOVES, Herve Jean Claude; FOLEY, Anne Marie; FOULKES, Gregory; JONES, Elizabeth Pearl; LECOMTE, Fabien Claude; QUINCEY, Joanna Rachel; SCHULZE, Monika-Sarah Elisabeth Dorothea; SELBY, Matthew Duncan; SMALLEY, Adam Peter; TAYLOR, Richard David; TOWNSEND, Robert James; ZHU, Zhaoning; (278 pag.)WO2018/229079; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com