Category: chlorides-buliding-blocks

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. 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C3H4Cl3NO

General procedure: Preparation of 2-methyl-6-nitro-2H-indazole (5d). To a stirred mixture of 6-nitro-1H-indazole (1.0 g, 0.0061 mmol) in dichloromethane (25.0 mL) was added trifluoromethanesulfonic acid (0.54 mL, 0.0061 mmol), stirred for 5-10 min at 25-35 C. To this mixture was added methyl 2,2,2,-trichlroacetimidate (2.69 g, 0.015 mmol) at room temperature. The reaction mixture was stirred at room temperature for 16-18 h under N2. After reaction completion, chilled saturated NaHCO3 solution was added. The aqueous and organic phases were separated. Aqueous phase was extracted with dichloromethane 10 mL. Combined organic layers were washed with DM water (2 × 10 mL). Organic layer was dried over anhydrous Na2SO4, filtered, and evaporated completely under vacuum to obtain 2-methyl-6-nitro-2H-indazole (1.03 g, 95.0%) as a yellow 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 2533-69-9.

Reference:
Article; Baddam, Sudhakar Reddy; Uday Kumar; Panasa Reddy; Bandichhor, Rakeshwar; Tetrahedron Letters; vol. 54; 13; (2013); p. 1661 – 1663;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 461432-23-5, These common heterocyclic compound, 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene, 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.

Under nitrogen, to a 50mL three-necked flask were added sequentially 3.99g2- chloro-5-bromo-ethoxy -4`- – diphenylmethane, 10ml of tetrahydrofuran and 30ml of toluene, followed by stirring to dissolve, cooled to -78 deg.] C, was added dropwise 2.4M n-hexane solution of n-butyllithium in 5.48ml, dropping the temperature was kept below -70 deg.] C, after the addition was complete the reaction was complete to give 2-chloro-5-ethoxy-lithium -4`- – diphenyl methane solution. Under nitrogen atmosphere, into a three-necked 250mL flask was added 8.43g Compound B-2 and 40ml of toluene, followed by stirring to dissolve, cooled to -78 deg.] C, the lithium-chloro-5-ethoxy -4`- – diphenylmethane was added dropwise, the dropping rate to keep the temperature below -65 deg.] C, after the addition was complete the reaction was kept 2 hours, 17.63g of tetrabutyl ammonium fluoride was added dropwise, the reaction was stirred for 1 hour at room temperature, methanol was added dropwise a solution of 7.45g of sulfuric acid ( containing 2.56 g of sulfuric acid), after the completion of the dropwise addition, the reaction mixture was stirred at room temperature, the HPLC monitoring of the reaction is complete, add saturated NaHCO3 solution to a pH of about 7.5, the organic layer was separated and the aqueous layer extracted with ethyl acetate, the combined organic phases were washed with saturated brine washed with water, vacuum distillation, additional 20ml toluene, evaporated under reduced pressure rotary evaporation to give 4.16g of intermediate -1, yield: 77.3%.

Statistics shows that 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene is playing an increasingly important role. we look forward to future research findings about 461432-23-5.

Reference:
Patent; Beijing Wan-sheng Pharmaceutical Co., Ltd.; Lin, Guoliang; Li, Xiaopeng; Liu, Zhidong; Wang, Zhanwei; Li, Yong; Pei, Yingzi; (15 pag.)CN105481915; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

1303587-99-6, name is 2-Chloro-7,8-dihydro-6H-pyrimido[5,4-b][1,4]oxazine, 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. Recommanded Product: 2-Chloro-7,8-dihydro-6H-pyrimido[5,4-b][1,4]oxazine

Synthesis of 2-chloro-8-(4-fluorobenzyl)-7 , 8-dihydro-6H-pyrimido [5, 4-b] [I, 4] oxazine [0440] To a stirred solution of 2-chloro-7, 8-dihydro-6H-pyrimido [5, 4-b] [1, 4] oxazine (100 mg, 0.58 mmol) in DMF (1 mL) under argon atmosphere was added sodium hydride (27 mg, 1.16 mmol) at 0 C. After stirring for 10 mins, l-(bromomethyl)-4-fluorobenzene (132 mg, 0.70 mmol) was added at 0 C and stirred for 1 h. After consumption of the starting materials (monitored by TLC), the reaction was quenched with ice water (20 mL) and extracted with EtOAc (2 x 20 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo to afford 2-chloro-8-(4-fluorobenzyl)-7, 8-dihydro- 6H-pyrimido [5, 4-b] [1, 4] oxazine (150 mg, 92%) as an off-white solid. 1H-NMR (DMSO- d6, 400 MHz): delta 7.70 (s, 1H), 7.36 (t, 2H), 7.18 (t, 2H), 4.75 (s, 2H), 4.19-4.16 (m, 2H), 3.51- 3.48 (m, 2H); LCMS: 279.9 (M+1); (column; X-Select CSH C-18 (50 3.0 mm, 3.5 mupiiota); RT 3.59 min 0.05% Aq TFA: ACN; 0.80 mL/min); TLC: 60% EtOAc/hexane (R 0.5).

The synthetic route of 1303587-99-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FORUM PHARMACEUTICALS INC.; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; MCRINER, Andrew, J.; WO2015/66697; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 6940-78-9, 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. 6940-78-9, name is 1-Bromo-4-chlorobutane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 9; Preparation 7-CBQ by a Reaction of 7-HQ with 1-bromo-4-chlorobutane in 2-propanol in Presence of About 47% sodium hydroxide solution; A mixture of 7-hydroxy-3,4-dihydro-2(1H)-quinolinone (4 g, 0.024 mole) and 1-bromo-4-chlorobutane (8.6 ml, 12.75 g, 0.073 mole, 3 eq.) in 2-propanol (20 ml) was refluxed followed by addition of mixture of about 47% aqueous sodium hydroxide solution (2.5 g, 0.029 mole, 1.2 eq.) and 2-propanol (4 ml). Reflux was continued for 2 hours. The hot reaction mixture was filtered, and the solvent and an excess of 1-bromo-4-chlorobutane were removed to dryness in vacuum. 2-propanol (12.5 ml) was added to the residue thus obtained and the mixture was refluxed to obtain a solution, followed by addition of a solution of 47% aqueous sodium hydroxide to produce a pH of about 10-11. The mixture was set aside at 10-15 C. for 6 hours. A colorless precipitate was collected by filtration, washed with cold mixture of water and 2-propanol (1:3, 7 ml) and water (10 ml). The solid was dried under reduced pressure at 50 C. overnight to obtain 7-(4-chlorobutoxy)-3,4-dihydro-2(1H)-quinolinone (5.55 g) in 89.2% yield, having a purity of 98.2% (by HPLC).

The synthetic route of 1-Bromo-4-chlorobutane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Naddaka, Vladimir; Brand, Michael; Davidi, Guy; Klopfer, Eyal; Gribun, Irina; Arad, Oded; Kaspi, Joseph; US2006/79689; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 363-51-9, 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. 363-51-9 name is 2-Chloro-6-fluoroaniline, 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.

To 2-chloro-6-fluoroaniline (24.8 g, 165 mmol) in HOAc (90 mL) is added Ac2O (18 mL, 189 mmol) and the mixture is stirred at 90 C. for 1 h. After cooling to rt H2O is added and the mixture is neutralized with 2 M NaOH solution with stirring. The aqueous layer is extracted twice with DCM. The combined organic layer is washed with semi-saturated NaHCO3 solution and brine, dried over MgSO4 and evaporated to give the acetanilide which is used without further purification

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-6-fluoroaniline, and friends who are interested can also refer to it.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2012/322803; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 202197-26-0, 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. 202197-26-0, name is 3-Chloro-4-((3-fluorobenzyl)oxy)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of 14 (1.03 g, 5 mmol), 10 mL SOCl2 and five drops of DMF was stirred and refluxed for 6 h. Excess SOCl2 was removed under reduced pressure, gave the intermediate 15 without further purification. A mixture of intermediate 15 and aniline (5 mmol) dissolved in 15 mL isopropanol, 1 mL Et3N was added, the mixture was stirred at reflux for 4 h. the reaction mixture was allowed to cool to room temperature. The precipitate was collected and washed with isopropanol, water and ether in order, dried to provide the products 16a-c.

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-((3-fluorobenzyl)oxy)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Li, Ri-Dong; Zhang, Xin; Li, Qiao-Yan; Ge, Ze-Mei; Li, Run-Tao; Bioorganic and Medicinal Chemistry Letters; vol. 21; 12; (2011); p. 3637 – 3640;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 102-49-8, name is 3,4-Dichlorobenzylamine, belongs to chlorides-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 102-49-8, Application In Synthesis of 3,4-Dichlorobenzylamine

A mixture of 3,4-dichlorobenzylamine (440 mg, 2.5 mmol) and acrylimide (185 mg, 2.6 mmol) was treated with silicon tetrachloride (6 mul, 0.05 mmol) under solvent-free conditions at 0°C. The mixture was heated to 60°C and stirred for 4 hr. The reaction was allowed to cool to rt and ethyl acetate (20 mL) and water (20 mL) were added. The layers were separated and the aqueous layer was further extracted with ethyl acetate (2 x 20 mL) and the combined organic layers were dried over sodium sulfate and concentrated in vacuo. The crude product was purified by flash column chromatography eluting with a gradient of dichloromethane: methanol (95:5 ? 85:15) to yield the product as a white solid (378 mg, 61percent).

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, 3,4-Dichlorobenzylamine, other downstream synthetic routes, hurry up and to see.

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

Reference of 19752-55-7,Some common heterocyclic compound, 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, molecular formula is C6H3BrCl2, 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.

It was dissolved in I-2 (68 g, 140 mmol) in a nitrogen environment in 500 mL tetrahydrofuran (THF), where the 1-bromo-3, 5-dichlorobenzene (38.0 g, 168.1 mmol) and tetrakis( triphenylphosphine) palladium was stirred into the (1.62 g, 1.4 mmol). Into a potassium carbonate (48.4 g, 350 mmol) in saturated water it was heated to reflux at 80°C for 12 hours. After the reaction was completed, the reaction solution into water and extracted with dichloromethane (DCM) and then water was removed with anhydrous MgSO4, filter and was concentrated under reduced pressure. Thus separated and purified the resulting residue was purified by flash column chromatography gave Compound I-3 (61.4 g, 87percent).

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

Reference:
Patent; Cheil Industries Co., Ltd; Lee, Han Ir; Yu, Uhn Sun; Kang, Dong Min; Kang, Uii Soo; Yang, Yong Tak; Oh, Jae Jin; Yu, Dong Gyu; Lee, Sang Sin; Jang, Yuna; Jung, Su Young; Han, Su Jin; Hong, Jin Suk; (59 pag.)KR2015/6758; (2015); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 19752-55-7, The chemical industry reduces the impact on the environment during synthesis 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, I believe this compound will play a more active role in future production and life.

N*3*-(3,5-Dichloro-phenyl)-l,N*5*-bis-(4-methoxy-benzyl)-N*5*-methyl-lH- [l,2,4]triazole-3,5-diamine In a 25 mL sealed tube, sodium tert-butoxide (97.9 mg, 1.02 mmol, Eq: 1.20), bis(dibenzylideneacetone)palladium (48.8 mg, 84.9 muiotaetaomicron, Eq: 0.1) and 2-di-tert-butylphosphino- 2′,4′,6′-triisopropylbiphenyl (36.0 mg, 84.9 muiotaetaomicron, Eq: 0.1) were combined with toluene (5 mL) to give a dark brown suspension. N5,l-bis(4-methoxybenzyl)-N5-methyl-lH-l,2,4-triazole-3,5- diamine (300 mg, 849 muiotaetaomicron, Eq: 1.00) and l-bromo-3,5-dichlorobenzene (230 mg, 1.02 mmol, Eq: 1.20) were added. The reaction mixture was degassed with argon for 15 min, and then heated to 110°C for 3 hours. The reaction mixture was cooled and diluted with EtOAc (50 mL), washed with H20 (25 mL) and brine (25 mL). The organic layer was dried over anhydrous MgS04, filtered and volatiles were removed under reduced pressure to yield an oil from which the compound was isolated by column chromatography (Hexanes/EtOAc = 70/30) to give an off- white solid 140 mg (33percent). MH+ 498.2

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, 1-Bromo-3,5-dichlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; DING, Qingjie; JIANG, Nan; WEIKERT, Robert James; WO2014/135472; (2014); A1;,
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. 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, This compound has unique chemical properties. The synthetic route is as follows., Safety of Methyl 2,2,2-trichloroacetimidate

500 mg (2.31 mmol) 3,4-diamino-benzene-sulfonylethan-2-ol were dissolved in 10 ml concentrated acetic acid. 0.4 ml (1.4 equiv.) methyl-2,2,2-trichloroacetimidate were added slowly and the resulting mixture was stirred at room temperature for 4 h. The mixture was diluted with 100 ml toluene and the solvent was removed under reduced pressure. The residue was rinsed with toluene, filtered and dried under vacuo to give a brown crystalline solid pure enough for all further reactions. Yield: 680 mg MS (ES+): m/e = 345, chloro pattern.

According to the analysis of related databases, 2533-69-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Aventis Pharma Deutschland GmbH; EP1479676; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics