Month: May 2021

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. 90390-33-3, name is 3-Chloro-5-fluorobenzylamine, A new synthetic method of this compound is introduced below., Recommanded Product: 90390-33-3

159 mg of 3-chloro-5-fluorobenzylamine (1 mmol) was weighed into a dry 50 mL eggplant-shaped reaction flask, and 15 mL of dichloromethane was added.The mixture was stirred until the substrate was completely dissolved. After adding 200 muL of triethylamine, a solution of 194 mg of octanoyl chloride (1.2 mmol in a suitable amount of dry dichloromethane) was slowly added dropwise under an ice bath at 0 to 5 C.After the completion of the dropwise addition, the TLC tracking and monitoring were carried out at room temperature, and when the raw materials disappeared, 20 mL of saturated sodium hydrogencarbonate was sequentially used.The water and the saturated aqueous NaCl solution were each washed three times and dried over anhydrous sodium sulfate.After vacuum distillation under reduced pressure, silica gel column chromatography was used to give N-(3-chloro-5-fluorobenzyl)octanamide.

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; Shanghai Shidande Biological Co., Ltd.; Shanghai Shidande Criterion Technology Services Co., Ltd.; Qian Yong; Xin Zhenqiang; Shu Yaping; Zhang Tianyong; Xie Tianpei; (11 pag.)CN108503559; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 81067-41-6 as follows. HPLC of Formula: C6H2Br2Cl2

Insert the 1,3-dibromo-2,5-dichlorobenzene (3.0g, 0.010mol) in pyridin-3-ylboronic acid (2.9g, 0.024mol) by synthesis by the same method used in Preparation Example 1-7 to give the intermediate 20-1> 2.1g (70% yield).

According to the analysis of related databases, 81067-41-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PNH TECH; HYUN, SEO YONG; JUNG, SUNG OUK; KIM, IK HWAN; (101 pag.)KR2016/40826; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 25186-47-4 as follows. Quality Control of 3,5-Dichlorotoluene

(1) device: Referring to Figure 2 to determine the connection of the tubular reactor, the pipeline type is:(3a + 3d) DC-channel+ enhanced hybrid round cake rectangular flat pipe,Pipe diameter and volume based on the flow rate and reaction to determine the residence time,Heat transfer medium for thermal oil.(2) 6.06 g of cobalt acetate and 6.06 g of sodium molybdate were dissolved respectively200ml3,5 – dichloro toluene and200ml acetic acid to form a mixed solution,In this case, n (cobalt acetate): n (3,5-dichlorotoluene) = 0.015: 1,6.06 g of sodium bromide was dissolved in 20% H2O2 to form a H2O2-acetic acid solution, where n (sodium bromide): n (3,5-dichlorotoluene) = 0.015: 1,3,5-dichlorotoluene-acetic acid Solution and andH2O2-acetic acid solution respectively to 8.33ml / min andThe flow rate of 16.67 ml / min was injected into the tubular reactor which was continuously heat-exchanging by the constant current pump, at this time, n (H2O2): n (3,5-dichlorotoluene) = 2:Using the microchannel reactor of Figure 2,The reaction temperature was controlled at 105 C and the residence time was 600 s.The outlet was cooled at 0 C and the reaction quenched with dichloromethane.After GC analysis, 3,5-dichlorotoluene conversion rate of 60.8%The yield of 3,5-dichlorobenzaldehyde was 39.2%.

According to the analysis of related databases, 25186-47-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Changzhou University; Yan Shenghu; Jiang Xin; Zhang Yue; Liu Jianwu; Shen Jiefa; Ma Xiaoming; Chen Daixiang; Gu Shunlin; Ni Fengchao; Li Yanfei; Wang Qiuhong; Chen Mingzhu; Wei Jin; Wu Fei; Zhang Yongchao; (9 pag.)CN106588606; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 467435-07-0,Some common heterocyclic compound, 467435-07-0, name is 4-Bromo-2-chlorobenzotrifluoride, molecular formula is C7H3BrClF3, 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.

Into a glass reaction vessel equipped with a stirrer and having a capacity of 250 mL,7.2 g (68.0 mmol) of sodium carbonate,2.6 g (20.4 mmol) of 2-thiopheneboronic acid,4-Bromo-2-chlorobenzotrifluoride 2.5 mL(17.0 mmol), dehydrated toluene 102 mL, dehydrated ethanol 51 mL,And 2.0 g (1.7 mmol) of tetrakistriphenylphosphine palladium,And the mixture was reacted at 80 C. for 16 hours.Water was added to the reaction product, and the mixture was extracted with methylene chloride.After drying with magnesium sulfate and distilling off the solvent under reduced pressure, purification by silica gel column chromatography (hexane) gave 4.4 g of compound (C11-c) as a white solid.

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-2-chlorobenzotrifluoride, its application will become more common.

Reference:
Patent; Ube Industries Ltd; Tanaka, Yasuhiro; Homma, Takashi; (66 pag.)JP2018/168138; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 622-98-0, These common heterocyclic compound, 622-98-0, name is 1-Chloro-4-ethylbenzene, 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.

2,5-Dichloro-2,5-dimethylhexane (compound 2) was synthesized using a known procedure set forth in Bruson H et al., J Am Chem Soc, 62:36 (1940), whereby 50 g of 2,5-dimethylhexane-2,5-diol (compound 1 ) and 1 L of concentrated hydrochloric acid was used. Yield was measured quantitatively. Properties of compound 2 matched that reported in Bruson et al.

Statistics shows that 1-Chloro-4-ethylbenzene is playing an increasingly important role. we look forward to future research findings about 622-98-0.

Reference:
Patent; WISCONSIN ALUMNI RESEARCH FOUNDATION; WO2007/5568; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 102170-53-6, name is 4-Bromo-5-chloro-2-methoxyaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 4-Bromo-5-chloro-2-methoxyaniline

Preparation of 2-(5-chloro-2-methylbenzoxazol-6-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (4) Preparation of 2-amino-5-bromo-4-chlorophenol (2): To a suspension of 4-bromo-3-chloro-6-methoxyaniline (1) (944 mg, 4 mmol) in 10 ml DCM was added 1 M BBr3 in DCM (8 ml, 8 mmol). The reaction mixture was stirred at r.t. for 2 h, which turned to a brown solution and back to a brown suspension. After quenched with aq. sodium bicarbonate solution, the mixture was extracted with EA. The org. phase was washed with brine, dried over sodium sulfate, concentrated to dryness to give 865 mg 2 as brown solid. Yield: 97.2%, purity>95%.

The synthetic route of 102170-53-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CalciMedica, Inc.; US2012/53210; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 2162-98-3, These common heterocyclic compound, 2162-98-3, name is 1,10-Dichlorodecane, 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.

5.68 g (0.05 M) of 4-chloropyridine was dissolved in 50 mL of dimethylformamide, and 15.63 g (0.025 M) of 1,10-dichlorodecane was separately dissolved in 170 mL of dimethylformamide. The 4-chloropyridine solution And the reflux reaction was carried out at 150 DEG C for 20 hours while slowly dropping at 100 DEG CWhen the thin layer chromatography phase reaction is completed, the reaction is stopped by adding about 20 mL of boiling water while cooling the reaction solution. The resulting solution is cooled to 0 C, made alkaline with 35% sodium hydroxide solution and extracted with dichloromethane doThe organic layer was washed with water and then magnesium sulfate was added to remove the water. The solution was distilled under reduced pressure to remove the solvent. 10.53 g of bis (4-chloropyridin-1 (4H) (Yield: 57.0%)

Statistics shows that 1,10-Dichlorodecane is playing an increasingly important role. we look forward to future research findings about 2162-98-3.

Reference:
Patent; Firson Co.,Ltd; Kim, Dong Jin; Koo, Chang Hwei; Park, Sung Yong; Cho, Ir Hwe; Lee, Sung Bae; Han, Dong Hoon; (12 pag.)KR2017/13425; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 320-60-5, 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. 320-60-5, name is 2,4-Dichloro-1-(trifluoromethyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

65 ml of 1.60 mol/1 of n-butyl lithium was slowly dropwise added at a temperature of from-75 to-65C over a period of 30 minutes to a solution of 14.8 ml of 2,4- dichlorobenzotrifluoride in 350 ml of anhydrous tetrahydrofuran, followed by stirring at-70C for 1 hour. At a temperature of from-75 to-65C, 15.9 ml of trimethyl borate was gradually dropwise added, followed by stirring for a while. Then, an ice bath was removed, and the mixture was stirred for 1 hour while gradually warming it to room temperature. Then, the reaction system was cooled to 0C, and 70 ml of ice water and 80 ml of 2N hydrochloric acid were gradually added with stirring, followed by stirring at room temperature overnight. Extraction with diethyl ether was carried out (300 ml x twice). The organic layers were put together, washed with a saturated sodium chloride aqueous solution and then dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. Suction drying was thoroughly carried. out to obtain 28 g of crude 2,6-dichloro-3-trifluoromethylbenzene boronic acid. This product was used as raw material for the next coupling reaction.

The synthetic route of 2,4-Dichloro-1-(trifluoromethyl)benzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ISHIHARA SANGYO KAISHA, LTD.?; WO2005/44007; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1009102-44-6, 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. 1009102-44-6 name is 1-(4-Chlorophenyl)cyclopropanamine hydrochloride, 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.

[00108] To a soution of (E)-3-((3aS,5aR,5bR,7aR,9S> 11 aR, 11 bR, 13aS)-9-hydroxy-1 – isopropyl-5a,5b,8,8,1 1 a-pentamethyl-2-oxo- 3,33,4,5,53,5^6,7,78,8,9,10,11 ,11a,11 b,12,13,13a-octadecahydro-2H- cyclopenta[a]chrysen-3a-yl)acrylic acid (500 mg, 1.007 mmol), 1-(4- chlorophenyl)cyclopropanamine hydrochloride (226 mg, 1.107 mmol) and HATU (765 mg, 2.013 mmol) in Nu,Nu-dimethylformamide (DMF) (2 ml_) stirred at 0C was added DIPEA (0.703 mL, 4.03 mmol) . The reaction mixture was stirred at 20 C for 1 h. The reaction mixture was adjusted pH to 3~4 by 2 M HCI, filtered, and the solid was washed with water (50 mL), solved into DCM, dried over sodium sulfate and evaporated in vacuo to give the crude product. The crude product was washed with petrol ether/EtOAc/DCM (10/1/1) to afford the target product (E)-N-(1-(4-chlorophenyl)cyclopropy)-3- ((3aS,5aR,5bR,7aR,9S, 11 aR, 1 1 bR, 13aS)-9-hydroxy-1 -isopropyl-5a,5b,8,8, 11 a- pentamethyl-2-oxo-3,3a,4, 5, 5a, 5b,6,7,7a,8,9, 10, 11 , 11 a, 1 1 b, 12, 13, 13a-octadecahydro-2H- cyclopenta[a]chrysen-3a-yl)acrylamide (685 mg, 1.007 mmol, 100 %)) as a yellow soild.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-(4-Chlorophenyl)cyclopropanamine hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; GLAXOSMITHKLINE LLC; HAN, Nianhe; JOHNS, Brian, A.; TANG, Jun; WO2013/91144; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 102170-53-6, 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. 102170-53-6 name is 4-Bromo-5-chloro-2-methoxyaniline, 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.

Preparation of 2-amino-5-bromo-4-chlorophenol (29): To a suspension of 4-bromo-3-chloro-6-methoxyaniline (28) (944 mg, 4 mmol) in 10 ml DCM was added 1 M BBr3 in DCM (8 ml, 8 mmol). The reaction mixture was stirred at r.t. for 2 h, which turned to a brown solution and back to a brown suspension. After quenched with aq. sodium bicarbonate solution, the mixture was extracted with EA. The org. phase was washed with brine, dried over sodium sulfate, concentrated to dryness to give 865 mg of 29 as a brown solid. Yield: 97.2%, purity>95%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-5-chloro-2-methoxyaniline, and friends who are interested can also refer to it.

Reference:
Patent; CalciMedica, Inc.; US2011/263612; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics