Author: Jessica.F

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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, A new synthetic method of this compound is introduced below., Application In Synthesis of 1-Bromo-3,5-dichlorobenzene

Under a nitrogen atmosphere, tert-butyllithium (1.3 Msolution in Pentane, 17.8 mL, 23.2 mmol) was added dropwise to a solution of 3,5-dichlorobromobenzene (5.0 g,22.1 mmol) in tetrahydrofuran (50 mL) dropwise over 30 min. The mixture was stirred for 2 hours and then N-methoxy-N-Methyl-2,2,2-trifluoroacetamide (3.64 g, 23.2 mmol) was added dropwise to the mixed solution, the reaction 2 was stirred while maintaining -78 ° Chour. Remove the low temperature, the temperature gradually rose to room temperature, the reaction was maintained at room temperature for 8 hours. Saturated ammonium chloride solution (50 mL)The reaction was quenched and extracted with ether (20 mL & apos; 3). The organic phases were combined and washed with brine (20 mL & apos; 2)The phases were dried over anhydrous magnesium sulfate, filtered, the solvent was removed and the residue was distilled under reduced pressure to give a colorless transparent liquid 1 (1.56 g). Yield29percent.

The synthetic route of 19752-55-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jingmen Pharmaceutical Industry Technology Institute; Wang Yong; Li Liwei; Hu Jianmei; Gu Dongyun; Huang Daoyou; (12 pag.)CN107353189; (2017); A;,
Chloride – Wikipedia,
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Related Products of 13078-79-0, 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. 13078-79-0, name is 2-(3-Chlorophenyl)ethanamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 42; N3-[2-(3-Chlorophenyl)ethyl]-N1-(2,3-dihydro-lH-inden-2-yl)-V-(2-{[2-(4-hydroxy-2- oxo-2,3-dihydro-l,3-benzothiazol-7-yl)ethyl]amino}ethyl)-beta-alaninamide bis- trifluoroacetic acid salt; The acrylamide as prepared in Example 41 step ii) (200 mg) was dissolved in ethanol (15 ml), 3-chlorophenethylamine (160 mg) was added and the mixture was stirred at room temperature for 5 days. The solvents were removed in vacuo and the residue was purified by flash chromatography on silica using ethyl acetate (100%), changing to 1% 0.88010 ammonia and 10% methanol in ethyl acetate as the eluents. The residue was treated with hydrogen bromide 30 wt % solution in acetic acid (3 ml), and the mixture was stirred at room temperature for 2 h. Toluene (1 ml) was added to the reaction and all solvents were removed in vacuo (x3). The residue was purified by reverse phase HPLC (5-95% acetonitrile in aqueous TFA) to give the title compound (19 mg).I51H NMR 90C delta (DMSO) 7.34-7.27 (3H, m), 7.21 (3H, d), 7.14 (2H, s), 6.81 (IH, d), 6.72(IH, d), 4.73 (IH, t), 3.55 (2H, s), 3.21-3.11 (12H, m), 2.51 (2H, m), 2.95 (2H, m), 2.80(2H, t).MS (Multimode +) 579.2 [(M-salt)+H]+ 0

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-(3-Chlorophenyl)ethanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2008/75026; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 6579-54-0,Some common heterocyclic compound, 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, molecular formula is C6H3Cl3O2S, 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.

3. Preparation of N-(5,7-dimethoxy[1,2,4]triazolo-[1,5-a]pyrimidin-2-yl)-2,6-dichlorobenzene-sulfonamide (Compound 1) 2-Amino-5,7-dimethoxy[1,2,4]triazolo[1,5-a]-pyrimidine (0.75 g, 3.8 mmol) and 2,6-dichlorobenzene-sulfonyl chloride (1.86 g, 7.6 mmol) were mixed in dry acetonitrile (15 mL). To this mixture was added dry pyridine (0.61 mL) and dry DMSO (54 muL, 0.7 mmol). The mixture was allowed to stir at room temperature. After 24 hours, the solvent was removed in vacuo, the residue was partitioned between CH2Cl2 (300 mL) and 2N HCl and the solids were collected by vacuum filtration to give a white solid A. The CH2Cl2 was dried (MgSO4) and removed in vacuo to give a white solid B. Both HPLC and NMR indicated that solid A and B are product. The solids were combined to afford the product as a white powder (1.41 g, 92%). mp 211-213 C. Anal: Cacld for C13H11Cl2N5O4S: C, 38.63; H, 2.74; N, 17.33; S, 7.93; found: C, 38.11; H, 2.68; N, 16.83; S, 7.77. 1H NMR (DMSO-d6): delta 12.4 (bs, 1H); 7.64-7.54 (m, 3H); 6.26 (s, 1H); 4.07 (s, 3H); 3.88 (s, 3H).

The synthetic route of 6579-54-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Johnson, Timothy Calvin; VanHeertun, John Cord; Ouse, David George; Arndt, Kim Eric; Pobanz, Mark Ardrew; Walker, David Keith; US2002/111361; (2002); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 102-49-8,Some common heterocyclic compound, 102-49-8, name is 3,4-Dichlorobenzylamine, molecular formula is C7H7Cl2N, 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.

A solution of 5-(hydroxymethyl)furfural (300 mg, 2.38 mmol) in methanol (10 mL) was treated with 3,4-dichlorobenzylamine (539 mg, 3.06 mmol), and the mixture stirred at rt for 5 hr. Sodium borohydride (158 mg, 4.18 mmol) was then added, and the solution was left to stir for 1 hr. The methanol was removed in vacuo and the residue dissolved in water (30 mL) extracted with dichloromethane (30 mL). The aqueous layer was further extracted with dichloromethane (2 x 30 mL) and the combined organic layers were dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by flash column chromatography on aluminium oxide eluting with dichloromethane: methanol (98:2) to yield the product as an orange oil (635 mg, 93percent).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,4-Dichlorobenzylamine, its application will become more common.

Reference:
Article; Brear, Paul; North, Andrew; Iegre, Jessica; Hadje Georgiou, Kathy; Lubin, Alexandra; Carro, Laura; Green, William; Sore, Hannah F.; Hyvoenen, Marko; Spring, David R.; Bioorganic and Medicinal Chemistry; vol. 26; 11; (2018); p. 3016 – 3020;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 348-59-4, name is 2,5-Dichlorofluorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2,5-Dichlorofluorobenzene

General procedure: 1-hloro-2-fluoro-4-methylbenzene (1.00 g) was dissolved in TFA (10 mL). The solution was cooled to 0C, and then, fuming nitric acid (5.0 mL) was added dropwise thereto. The mixture was stirred at 0C for 30 minutes, and then, the solution was added to an aqueous sodium bicarbonate solution and neutralized, followed by extraction with chloroform. The extract was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel chromatography (hexane/ethyl acetate) to obtain 1.31 g of the title compound as a white solid.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 348-59-4.

Reference:
Patent; Taiho Pharmaceutical Co., Ltd.; IRIE, Hiroki; OGUCHI, Kei; FUJIOKA, Yayoi; EP3590516; (2020); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 2106-02-7,Some common heterocyclic compound, 2106-02-7, name is 2-Chloro-4-fluoroaniline, molecular formula is C6H5ClFN, 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.

A microwave tube was charged with 2-(9-bromo-4,5-dihydro-6-oxa-1-thia-benzo[e]azulen-2-yl)-[1,3,4]oxadiazole (0.64 g; 1.83 mmol), 2-chloro-4-fluoroaniline (0.44 ml; 3.68 mmol), TFA (0.27 ml; 3.63 mmol) and toluene (5 ml). The mixture was heated in a microwave at 160 C. for 30 min., diluted with EtOAc (150 ml) and washed with satd. NaHCO3. The organic layer was dried (MgSO4), concentrated and purified by ISCO to give 267 as a cream-coloured solid (0.59 g; 68%). deltaH (400 MHz, CDCl3) 3.14 (t, J=5.2, 2H), 4.29 (t, J=5.2, 2H), 6.91 (d, J=8.4, 1H), 6.93 (s, 1H), 7.22-7.27 (m, 2H), 7.43-7.51 (m, 2H), 7.65 (d, J=2.4, 1H), 8.22 (s, 1H). [M+H]+: 478

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

Reference:
Patent; Genentech, Inc.; US2009/247567; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

928782-97-2, name is 4-Chloro-2-(phenylethynyl)aniline, belongs to chlorides-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. name: 4-Chloro-2-(phenylethynyl)aniline

A mixture of 2-alkynylaniline 1a-1e (0.2 mmol), dichalcogenide 2a-2e (0.15 mmol), CuI (0.02 mmol), and Cs2CO3 (0.2 mmol) in DMSO (2 mL) was stirred at 80 C under an air atmosphere. After completion of the reaction that was monitored by GC-MS or TLC, 25 mL water was added, and the mixture was extracted with ethyl acetate, the combined organic layers were washed with water (10 mL x 3), dried over anhydrous Na2SO4. After filtration and removal of solvents in vacuum, the residue was purified by silica gel column chromatography to afford the corresponding products.

The synthetic route of 928782-97-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Li, Zhen; Hong, Longcheng; Liu, Ruiting; Shen, Jianzhong; Zhou, Xigeng; Tetrahedron Letters; vol. 52; 12; (2011); p. 1343 – 1347;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 41965-95-1, 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. 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

(3-Chloro-4-methoxyphenyl) methanamine hydrochloride compound of formula-6a (76.98 g) was added to the organic layer containing ethyl 4-chloro-2-(methylthio) pyrimidine-5-carboxylate compound of formula-5, which is obtained in step-b). Water (100 ml), followed by sodium carbonate (110.3 g) were added to the reaction mixture at 25-30C and stirred for 4 hours at the same temperature. After completion of the reaction, water was added to it. Both the organic and aqueous layers were separated; the aqueous layer was extracted with toluene. All the organic layers were combined and washed with water. Distilled off the solvent from the organic layer under reduced pressure. The reaction mixture was cooled to 30-35C. 700 ml of cyclohexane: ethyl acetate (in 9.5:5 ratio) was added to the reaction mixture. The reaction mixture was heated to 70-75C and stirred until complete dissolution. The reaction mixture was cooled to 10-15C and stirred for 3 hours. Filtered the precipitated solid, washed with cyclohexane and then dried to get title compound.Yield: 90 gms; Melting range: 81 -84C; Purity by HPLC: 95.3%.

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-Chloro-4-methoxybenzylamine Hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MSN LABORATORIES PRIVATE LIMITED; THIRUMALAI RAJAN, Srinivasan; ESWARAIAH, Sajja; SATYANARAYANA, Komati; WO2015/1567; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 1127-85-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1127-85-1 name is 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: To the solution of compounds 22 (0.3 g, 1.5 mmol) in DMF wereadded K2CO3 (1.95 mmol) and 4-amino-1-Boc-piperidine (2.7 mmol). The reaction was stirred at 80 C for 8 h. Then the mixture was extractedwith ethyl acetate, washed with brine, dried over MgSO4, andevaporated. The residue was purified by column chromatography togive the product (0.5 g, 92% yield).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline, and friends who are interested can also refer to it.

Reference:
Article; Fang, Yuanying; Xiong, Lijuan; Hu, Jianguo; Zhang, Shaokun; Xie, Saisai; Tu, Liangxing; Wan, Yang; Jin, Yi; Li, Xiang; Hu, Shaojie; Yang, Zunhua; Bioorganic Chemistry; vol. 86; (2019); p. 103 – 111;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 928782-97-2, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 928782-97-2 name is 4-Chloro-2-(phenylethynyl)aniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

General procedure: To a microwave vial, a mixture of 2-alkynylaniline (1 equiv), sulfonyl hydrazide (1.5 equiv), I2 (10 mol%) and pTSA (50 mol%) was taken in 1,4-dioxane irradiated for 15 min at 110C, 100W in CEM microwave synthesizer. The progress and completion of reaction is monitored by TLC using EtOAc/n-Hexane (1:10) as an eluent. The reaction mixture was then cooled to room temperature and extracted with ethyl acetate. The combined organic phase was washed with sodium thiosulphate (50 mL) and dried over Na2SO4. After filtration and evaporation of the solvents in vacuum, the mixture of products was separated by column chromatography on silica gel (EtOAc/n-hexane: 1:10) to yield the desired product 3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-2-(phenylethynyl)aniline, and friends who are interested can also refer to it.

Reference:
Article; Sharma, Shivani; Pathare, Ramdas S.; Sukanya; Maurya, Antim K.; Goswami, Bhagyashree; Agnihotri, Vijai K.; Sawant, Devesh M.; Pardasani, Ram T.; Tetrahedron Letters; vol. 58; 40; (2017); p. 3823 – 3826;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics