Month: March 2021

Related Products of 61881-19-4, A common heterocyclic compound, 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, molecular formula is C8H5ClF3N, 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.

General procedure: Add sodium acetate, trifluoroethylimidyl chloride (II), hydrazone (III), and 1 mL of organic solvent to the 35 mL Schlenk tube according to the raw material ratio in Table 1.Mix and stir well. After the reaction is completed according to the reaction conditions in Table 2, 2-4 hours,Add elemental iodine, continue the reaction for 1-2 hours, filter, and stir the sample in silica gel.After purification by column chromatography, the corresponding 5-trifluoromethyl-substituted 1,2,4-triazole compound (I) is obtained. The reaction process is shown by the following formula:

The synthetic route of 61881-19-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang Sci-Tech University; Chen Zhengkai; Hu Sipei; Yang Zuguang; (10 pag.)CN110467579; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 118-69-4, name is 2,6-Dichlorotoluene, A new synthetic method of this compound is introduced below., Application In Synthesis of 2,6-Dichlorotoluene

EXAMPLE 1-1 Preparation of 2,4-dichloro-3-methylbromobenzene To a solution of 48.8 g (0.3 mol) of 2,6-dichlorotoluene in 60 ml of carbon tetrachloride, 0.7 g of iron powder and 0.1 g of iodine were added. Then, 52.8 g (0.33 mol) of bromine was dropwise added thereto at room temperature while maintaining the reaction temperature at a level of from 22 to 25 C. After completion of the dropwise addition, the reaction was continued at the same temperature until generation of hydrogen bromide ceased. After the reaction, the reaction solution was added to 300 ml of ice water and extracted with 300 ml of 1,2-dichloroethane. The organic layer was separated and washed sequentially with water, a saturated sodium hydrogen sulfite aqueous solution, water and a saturated sodium chloride aqueous solution. Then, the solvent was distilled off under reduced pressure to obtain 71.9 g (yield: 99.5%) of desired 2,4-dichloro-3-methylbromobenzene. Melting point: 32-33 C.

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; Nissan Chemical Industries Ltd.; US4942246; (1990); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 6775-78-6, These common heterocyclic compound, 6775-78-6, name is 6-Chloroimidazo[1,2-b]pyridazine, 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.

A mixture of 6-chloro-imidazo[1,2-b]pyridazine (0.40 g, 2.6 mmol) and bromine (0.12 mL, 2.3 mmol) in methanol (20 mL) was stirred at room temperature. Evaporation of the reaction mixture gave 3-bromo-6-chloro-1-yl-imidazo[1,2-b]pyridazine as a yellow solid (0.69 g); this material was used in the next reaction without further purification: LC/MS [M+H]+ 232, 234.

The synthetic route of 6775-78-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ALCON MANUFACTURING, LTD.; US2008/153813; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 14752-66-0, 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. 14752-66-0, name is Sodium 4-chlorobenzenesulfinate belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of sodium arylsulfinates (1.0 mmol), nitroarenes (0.5 mmol), NaHSO3 (1.0 mmol), MIL-101(Fe) (10 mg, 8 mol% of Fe) in H2O (2 mL) were stirred at 60 oC for 20 h in a sealed tube. After cooling to room temperature, the aqueous solution was extracted with ethyl acetate (3 ¡Á 3 mL), and the combined extract was dried with anhydrous Na2SO4. The solvent was removed, and the crude product was separated by a flash chromatography on a silica gel column to afford the pure product 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, Sodium 4-chlorobenzenesulfinate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Li, Xinxin; Chen, Fei; Lu, Guo-Ping; Tetrahedron Letters; vol. 59; 48; (2018); p. 4226 – 4230;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 95-51-2, name is 2-Chloroaniline, 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 95-51-2, Safety of 2-Chloroaniline

General procedure: Into a pressure microreactor of stainless steel of 17 mL capacity or into a glass ampule (20 mL) (results of the parallel runs were virtually identic) was charged 5-10 wt % of catalyst (0.94HY-BS, NaY-BS, 0.72KNaX-BS), 100 mmol of aniline or its derivative, and 400 mmol of dimethyl carbonate. The reactor was hermetically closed (the ampule was sealed), and was heated for 1-4 h at 150 C. After the end of the run the reactor was cooled to room temperature, opened, the reaction mixture was filtered through a bed of Al2O3. Dimethyl carbonate was distilled off, the residue was distilled at atmospheric pressure or in a vacuum, or crystallized from ethanol.

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

Reference:
Article; Khusnutdinov; Shchadneva; Mayakova, Yu. Yu.; Ardieva; Khazipova; Kutepov; Russian Journal of Organic Chemistry; vol. 52; 11; (2016); p. 1565 – 1570; Zh. Org. Khim.; vol. 52; 11; (2016); p. 1574 – 1578,5;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 63624-28-2,Some common heterocyclic compound, 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, molecular formula is C8H9ClO4S, 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 1 3-Amino-5-chloro-1,3-dihydro-1-(2,4-dimethoxybenzenesulfonyl)-3-phenylindol-2-one A solution of 0.3 g of 3-amino-5-chloro-1,3-dihydro-3-phenylindol-2-one in 7 ml of DMF is cooled to 0 C. under an argon atmosphere and 0.037 g of sodium hydride as an 80% dispersion in oil is added. After stirring for 20 minutes, 0.275 g of 2,4-dimethoxybenzenesulfonyl chloride is added and the reaction mixture is stirred overnight, the temperature being allowed to rise to RT. It is poured into water, extracted with AcOEt, washed with water and with a saturated solution of NaCl, dried over sodium sulfate and evaporated under vacuum. The residue is chromatographed on silica using a DCM/AcOEt mixture (95/5; v/v) as the eluent to give the expected product after crystallization from a DCM/iso ether/hexane mixture. m=0.31 g. M.p.=108-110 C.

The synthetic route of 63624-28-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sanofi; US5594023; (1997); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 452-73-3, A common heterocyclic compound, 452-73-3, name is 2-Chloro-4-fluoro-1-methylbenzene, molecular formula is C7H6ClF, 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.

Step A Synthesis of 2-chloro-4-fluorobenzal bromide In a flask were placed 150 g (1.04 moles) of 2-chloro-4-fluorotoluene, 391 g (2.20 moles) of N-bromosuccinimide, 3 g (0.012 mole) of benzoyl peroxide, and 800 ml of carbon tetrachloride. This mixture was refluxed overnight and then filtered. The solvent was evaporated under reduced pressure, leaving a residue of impure 2-chloro-4-fluorobenzal bromide weighing 340 g.

The synthetic route of 452-73-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FMC Corporation; US4846875; (1989); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 118-69-4, 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. 118-69-4, name is 2,6-Dichlorotoluene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a round bottom flask was added 100 g of 2,6-dichlorotoluene, 0.5 g antimony trichloride, 59.6 g of chlorine gas was introduced at 25 C under atmospheric pressure, the reaction temperature was controlled at 25 to 30 C, Chlorine speed of 10g / h, After about 6 hours, the reaction of 2,6-dichlorotoluene was terminated by GC, and chlorine was stopped. 124.1 g of a reaction liquid was obtained, which comprised 85.4% of 2,3,6-trichlorotoluene, 1.9% of 2,4,6-trichlorotoluene, 12.7% of tetrachlorotoluene and impurities. The reaction solution was subjected to distillation to obtain 104.7 g of 2,3,6-trichlorotoluene in a yield of 86.3% GC area content of 98%.

The synthetic route of 2,6-Dichlorotoluene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Lianhua Technology Co., Ltd.; Lianhua Technology (Yancheng) Co., Ltd.; Fan, Xiaobin; Lin, Xingjun; Xu, Xiaoming; Huang, Chao; Chen, Donghua; Zhou, Shuyong; (8 pag.)CN105601466; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 821-10-3, name is 1,4-Dichlorobut-2-yne, A new synthetic method of this compound is introduced below., SDS of cas: 821-10-3

[0038] The 1 ,4-dichloro-2-butyne 14 of Example 2 is de-halogenated by base promoted elimination of HC1 to produce diacetylene 15. A mixture of 4 M aqueous potassium hydroxide (3 equivalents) and dimethyl sulfoxide (1 mL per 16 mmol potassium hydroxide) is heated to about 70-75 C. 1 ,4-dichloro-2-butyne (1 equivalent) is added slowly to the mixture while bubbling argon through the solution. The volatile product is directed through a series of two gas washing bottles containing dilute aqueous potassium hydroxide followed by two calcium chloride drying tubes and into a vessel containing anhydrous tetrahydrofuran cooled in an ice-calcium chloride bath to yield a tetrahydrofuran solution of diacetylene 15.

The synthetic route of 821-10-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EMPIRE TECHNOLOGY DEVELOPMENT LLC; KLEIN, Josef Peter; WO2015/60862; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 39226-95-4, 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. 39226-95-4, name is 2,3-Dichlorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 20: Preparation of N-(4,5-dihydrothiazol-2-yl)-N-[1-(2,3-dichlorophenyl)-3- methylbut-3-enyl]amine20.1 Preparation of N-(2,3-dichlorobenzyl)-N-(4,5-dihydrothiazol-2-yl)amineA solution of 2-chloroethyl isothiocyanate (3.45 g) in diethyl ether (20 ml) was added dropwise to a solution of 2,3-dichlorobenzylamine (5.00 g) in diethyl ether(80 ml) at 0 0C and the mixture was allowed to warm up to room temperature over 3 h. An aqueous solution of sodium hydroxide (1 M, 100 ml) was then added and the mixure was further stirred for 1 h. After seperation of the phases, the organic phase was washed with water, dried over sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography to yieldN-(2,3-dichlorobenzyl)-N-(4,5-dihydrothiazol-2-yl)amine.

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

Reference:
Patent; BASF SE; WO2009/115491; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics