Category: chlorides-buliding-blocks

50638-47-6, name is 4-Bromo-2-chloro-1-methoxybenzene, 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. Quality Control of 4-Bromo-2-chloro-1-methoxybenzene

To a 3-necked round bottom flask was added 4-bromo-2-chloro-1-methoxy-benzene(45.00 g, 203.18 mmol) and THF (450 mL), n-Butyllithium (2.5 M in hexanes, 90.21 mL, 1.11 eq) was added at -78 C. The mixture was stirred for 2 h at -78 C. A solution of 1,4- dioxaspiro[4.5]decan-8-one (34.91 g, 223.50 mmol) in THF (90 mL) was added dropwise to the reaction mixture. The resulting mixture was stirred for 3 h at -78 C. The reaction was quenched with aqueous NH4C1 (lOOmL) and extracted with EtOAc (500 mL). The organic layer was dried (Na2504), filtered and concentrated. The residue was washed with hexanes (350 mL), filtered and dried under high vacuum. The solid was triturated with hexanes (15 mL), filtered and dried under high vacuum to give 8-(3-chloro-4-methoxy-phenyl)-1,4- dioxaspiro[4.5]decan-8-ol (37 g, 61%) as a white solid. ?H NMR (400 IVIHz, CDC13): 7.31 (d, 1H), 7.29 (dd, 1H), 7.10 (d, 1H), 3.90-3.92 (m, 4H), 3.89 (s, 3H), 1.99-2.02 (m, 4H), 1.70- 1.73 (m, 4H); LCMS: 281.2 [M-OH].

The synthetic route of 50638-47-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; METACRINE, INC.; SMITH, Nicholas D.; GOVEK, Steven P.; NAGASAWA, Johnny Y.; (169 pag.)WO2018/170166; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 50594-82-6, name is 3,4,5-Trichlorobenzotrifluoride, molecular formula is C7H2Cl3F3, 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. HPLC of Formula: C7H2Cl3F3

Comparative Example 3: Preparation of 2,6-dichloro-4-(trifluoromethyl)phenyl- hydrazine of the formula 1-1 from 3,4,5-trichloro- benzotrifluoride in toluene; 10 g (40 mmole) of 3,4,5-trichlorobenzotrifluoride (99.7% purity) were dissolved in 30 g (326 mmole) of toluene. To this solution were added 8 g (160 mmole) of hydrazine hydrate (100%). The resulting mixture was stirred at reflux (approx. 1100C) for 24 hours. Thereafter, an organic phase of 39.4 g was separated. The solution obtained by this separation contained the product 2,6-dichloro-4-(trifluoromethyl)phenylhydrazine in an amount of 0.9 wt-% and the starting material 3,4,5-trichlorobenzotrifluoride in an amount of 26.3 wt-%, meaning that a product yield not higher than 3.6 % was obtained.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 50594-82-6, its application will become more common.

Reference:
Patent; BASF SE; WO2008/113661; (2008); A2;,
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

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

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

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 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

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

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

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