Month: September 2021

Adding a certain compound to certain chemical reactions, such as: 33184-48-4, name is 4-Chloro-2-iodo-1-methylbenzene, 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 33184-48-4, Formula: C7H6ClI

The boronate ester (1.0 equiv), iodo-benzene (1.0 equiv), palladium catalyst (0.1 equiv) and potassium carbonate (3.0 equiv) was added to a solution of deoxygenated DMF. The flask was flushed with argon for 15 minutes, fitted with a dry tube and run over night at 110 0C. The reaction was poured onto water and extracted three times with ethyl acetate. The organic layers were washed with a brine solution, dried over anhydrous sodium sulfate. The reaction was purified through a 10 g SPE tube in a mixture of ethyl acetate and hexanes. IH NMR was used to confirm the purity of the product.; 4-(5-Chloro-2-methyl-phenyl)-3,6-dihydro-2H pyridine- 1-carboxylic acid tert-butyl ester was synthesized from 4-(4,4,5,5-tetramethyl-[l,3,2]dioxaborolan-2-yl)-3,6-dihydro-2H-pyridin-l- carboxylic acid tert-butyl ester ( 0.200 g, 0.647 mmol), 4-chloro-2-iodo-l -methyl-benzene ( 0.163 mg, 0.647 mmol), Pd Cl2 (dppf) (0.053 g, 0.0647 mmol) and potassium carbonate (0.268 g, 1.94 mmol) in 20.0 mL of DMF. The reaction was purified by eluting through a 10 g SPE tube using a solution of 10% ethyl acetate and hexanes to yield a brown liquid (0.236 g, 124%). 1H NMR (300 MHz, CDC3) delta ppm: 1.54 (s, 9H), 2.02 (s, 2H), 2.39 (s, 3H), 3.66 (br, 2H), 4.15-4.06 (br, 2H), 5.52 (br, IH), 7.78-7.07 (m, 3H).

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; ASTRAZENECA AB; NPS PHARMACEUTICALS, INC.; WO2006/71730; (2006); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

627-32-7, name is 3-Iodo-1-propanol, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 3-Iodo-1-propanol

To a solution of 5-bromo-1, 2-dihydropyridin-2-one (1 g, 5.75 nMol, 1 equiv) and 3-iodopropan-1-ol (2.1 g, 11.49 nMol, 2 equiv) in DMF (15 mL) was added K 2CO 3 (1.6 g, 11.49 nMol, 2 equiv) at room temperature. The mixture was stirred for 4 hours at 80 under air atmosphere. The resulted mixture was concentrated under reduced pressure. The residue was purified by Prep-TLC (CHCl 3 /MeOH 20: 1) to afford 5-bromo-1- (3-hydroxypropyl) -1, 2-dihydropyridin-2-one (300 mg, 22.49%) as a yellow solid. LCMS: m/z (ESI) , [M+H] + = 232.1, 234.1. 1H NMR: (300 MHz, DMSO-d 6) delta 1.12 (q, 2H) , 2.79 (m, 2H) , 3.27 (t, 2H) , 4.03 (s, 1H) , 5.69 (d, 1H) , 6.78 (dd, 1H) , 7.09 (d, 1H) .

The synthetic route of 627-32-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DIZAL (JIANGSU) PHARMACEUTICAL CO., LTD.; QI, Changhe; TSUI, Honchung; ZENG, Qingbei; YANG, Zhenfan; ZHANG, Xiaolin; (399 pag.)WO2020/35052; (2020); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

31599-60-7, name is 1-Iodo-2,3-dimethylbenzene, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C8H9I

General procedure: A suspension of indole-3-carbaldehyde 1 (0.411 g, 2.8 mmol),Cu2O (0.3 equiv), K2CO3 (2.0 equiv) and aryl halide (2.0 equiv) inanhydrous DMF (5.6 mL) was refluxed for 72 h. After cooling to RT,the reaction mixture was filtrated over a celite pad eluting withEtOAc. Solvents were removed and the residue dissolved in EtOAc(20 mL) washed successively by 2.5% aqueous NH4OH, 1 M HCl andsaturated aqueous NaCl. The organic phase was dried over Na2SO4,filtered and concentrated. The residue was purified by flash columnchromatography on silica gel (PE/EtOAc 9:1 to 7:3) to furnish thedesired compound.

The synthetic route of 31599-60-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sagnes, Charlene; Fournet, Guy; Satala, Grzegorz; Bojarski, Andrzej J.; Joseph, Benoit; European Journal of Medicinal Chemistry; vol. 75; (2014); p. 159 – 168;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 16355-92-3, The chemical industry reduces the impact on the environment during synthesis 16355-92-3, name is 1,10-Diiododecane, I believe this compound will play a more active role in future production and life.

2-Picoline (0.30 mL, 3.1 mmol) and 1,10-diiododecane (13.0 g, 33 mmol) were dissolved in acetone (20 mL) with a 50 mL flask equipped with a condenser. The solution was heated to reflux at 60C for 4 days. The solution was dropped into hexane (300 mL), and then a yellow precipitate was obtained. The precipitate was recovered and dried to obtain the product 4 as yellow powder (yield 1.3 g, 87%). 1H NMR (500MHz, DMSO-d6): delta 8.96 (d, J=5.1Hz, 1H), 8.44 (t, J=7.8Hz, 1H), 8.02 (d, J=7.9Hz, 1H), 7.94 (t, J=6.8Hz,1H), 4.51 (t, J=7.8Hz, 2H), 3.25 (t, J=6.8Hz, 2H), 2.82 (s, 3H), 1.85-1.79 (m, 2H), 1.75-1.69 (m, 2H), 1.36-1.22 (m, 12H).

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, 1,10-Diiododecane, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Hashidzume, Akihito; Kuse, Akihiro; Oshikiri, Tomoya; Adachi, Seiji; Yamaguchi, Hiroyasu; Harada, Akira; Tetrahedron; vol. 73; 33; (2017); p. 4988 – 4993;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding a certain compound to certain chemical reactions, such as: 3718-88-5, name is 3-Iodobenzylamine hydrochloride, 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 3718-88-5, COA of Formula: C7H9ClIN

A suspension of 3-iodobenzylamine hydrochloride (4.95g, 18.4mmol) in dichloromethane (100ml) was treated with triethylamine (3.1ml, 22mmol) and di-t-butyl dicarbonate (4.40g, 20mmol) and the resulting solution left to stir at room temperature under a nitrogen atmosphere for 1.5 hours. The reaction mixture was washed with 2M hydrochloric acid (30ml), water (30ml), dried (sodium sulfate), and the solvent removed in vacua to give the title compound as a colourless solid (6.43g).1HNMR (400MHz, CDCI3) 5 :7.63 (s, 1H), 7.60 (d, 1H), 7.25 (d, 1H), 7.06 (dd, 1H), 4.79-4.89 (bs, 1H), 4.21-4.30 (m, 2H), 1.46 (s, 9H) ppm.MS (electrospray) m/z 332 [M-H]’, 356 [M+Na]”1″

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-Iodobenzylamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2004/108676; (2004); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Related Products of 2142-70-3,Some common heterocyclic compound, 2142-70-3, name is 1-(2-Iodophenyl)ethanone, molecular formula is C8H7IO, 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.

l-(2-{[(4alphaS,5R)-l-(4-Fluorophenyl)-5-hydroxy-4alpha-methyl-l,4,4alpha,5,6,7- hexahydrocyclopenta[f]indazol-5-yl]ethynyl}phenyl)ethanone (8-1). Diisopropylamine (0.924 ml, 6.49 mmol) was added to a solution of 1-6 (2.0 g, 6.49 mmol), l-(2-iodophenyl)ethanone (l-91g, 7-78 mmol), bis(triphenylphosphine)palladium (II) 5 chloride (228 mg, 0.324 mmol), and CuI (62 mg, 0.324 mmol) in anhydrous THF (20 ml) at ambient temperature. The resulting solution was stirred at ambient temperature for 18 hours, then diluted with diethyl ether, filtered through a pad of celite and the solvent removed in vacuo. Purification by flash chromatography on 120 g of silica, eluting with a gradient of 0-100% EtOAc in hexanes afforded 2.6 g, 94 % of 8-1 as an orange oil. 10 MS (ESI): m/z = 427.22 (MH+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-(2-Iodophenyl)ethanone, its application will become more common.

Reference:
Patent; MERCK & CO., INC.; WO2008/51532; (2008); 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. 148870-57-9, name is 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one, A new synthetic method of this compound is introduced below., Recommanded Product: 7,8-Dimethoxy-3-(3-iodopropyl)-1,3-dihydro-2H-3-benzazepin-2-one

A mixture of (S)-N- [(4,5 -dimethoxybenzocyclobut- 1 -yl)methyl] -N-(methyl)amine hydrochloride (lOOg) and d.imethyl formamide (400mL) was stirred for about 5mm and potassium carbonate (178.46g) was added to it. The reaction mixture was stirred forabout lh at about room temperature. The reaction mixture was cooled to about 5C to about 10C. 7, 8-dimethoxy-3 -[3 -iodopropyl] – 1,3 -dihydro-2H-3 -benzazepin-2-one (3 6g) prepared as in Example 8, was added to the stirred reaction mixture. The reaction mixture was stirred for about 4h at about 20C to about 25C. The reaction mixture was quenched into chiHed demineralized water at about 5C to about 10C. The reaction mixture wasacidified to pH of about I to about 2 using concentrated hydrochloric acid and ethyl acetate was added to it. The reaction mixture was stirred and the two layers were separated. The aqueous layer was basified to pH of about 8 to about 9.5 using 20-25% aqueous ammonia solution and ethyl acetate was added to it. The reaction mixture was stirred and the two layers were separated. The organic layer was washed withdemineralized water and concentrated under reduce pressure at about below 55C.Yield: 75%; HPLC purity: > 96%

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; GLENMARK PHARMACEUTICALS LIMITED; GLENMARK GENERICS LIMITED; BHIRUD, Shekhar Bhaskar; BHUSHAN, Kumar Hari; ZOPE, Sunil Sudhakar; PATIL, Dipak Vinayak; DHEBADE, Pramod Amrutrao; CHAND, Prem; WO2014/102827; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 112671-42-8,Some common heterocyclic compound, 112671-42-8, name is 4-Bromo-1-iodo-2-nitrobenzene, molecular formula is C6H3BrINO2, 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.

(1) In the reaction bottle, add N-phenylcarbazole-4-boronic acid (100mmol), 2-iodo-5-bromonitrobenzene (100mmol), 0.9g (0.785mmol, 0.5%) tetratriphenylphosphine Palladium, toluene 500mL, ethanol 200mL, water 200mL, and potassium carbonate 40g (300mmol), react at 100 C for 8h; after the reaction is complete, stop the reaction; cool to room temperature, separate the organic phase, concentrate, silica gel column chromatography to obtain yellow powder M1;

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Bromo-1-iodo-2-nitrobenzene, its application will become more common.

Reference:
Patent; Yantai Xianhua Chemical Technology Co., Ltd.; Xing Qifeng; Feng Peichuan; Chen Yue; Hu Lingfeng; Chen Yili; (24 pag.)CN110734446; (2020); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 5876-51-7,Some common heterocyclic compound, 5876-51-7, name is 5-Iodobenzo[d][1,3]dioxole, molecular formula is C7H5IO2, 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.

General procedure: A 100mL flask was charged with Pd(PPh3)Cl2 (70 mg, 0.1 mmol) and CuI (38 mg, 0.2 mmol). After the flask was evacuated and refilled with argon, NEt3 (20 mL) was added and the suspension was stirred at room temperature. A solution of iodobenzene (10a, 2.04 g, 10 mmol) and propargyl alcohol (616 mg, 11 mmol) in NEt3 (10 mL) was added to the suspension. After the reaction was complete (monitored by TLC), the mixture was filtered through a plug of Celite and washed with EtOAc (20 mL x 3). The combined solution was concentrated and purified by column chromatography on silica gel (Hexane/EtOAc 3:1, v/v) to afford 3-phenylprop-2-yn-1-ol (11a, 1.24 g, 94% yield) as a yellow oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Iodobenzo[d][1,3]dioxole, its application will become more common.

Reference:
Article; Xu, Bin; Gartman, Jackson A.; Tambar, Uttam K.; Tetrahedron; vol. 73; 29; (2017); p. 4150 – 4159;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 13421-13-1, A common heterocyclic compound, 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, molecular formula is C7H4ClIO2, 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.

Example 3Amethyl 4-chloro-2-iodobenzoate To a solution of 4-chIoro-2-iodobenzoic acid (10.61 g, 37.62 mmol) in methanol (75 ml), trimethylsilyldiazomethane (30 ml, 2.0 M in ether) was added drop by drop. 1725 After 1 hour, another batch of trimethylsilyldiazomethane (26 ml, 2.0 M in ether) was added drop by drop. The reaction mixture was stirred at room temperature overnight and concentrated. The crude product was purified by column chromatography (0-20% ethyl acetate in hexanes) to yield the title compound.

The synthetic route of 13421-13-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBOTT LABORATORIES; ABBOTT LABORATORIES TRADING(SHANGHAI) COMPANY, LTD.; VAN CAMP, Jennifer; PATEL, Jyoti, R.; SWANN, Steven; WO2012/45194; (2012); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com