Month: September 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. 106-39-8, name is 1-Bromo-4-chlorobenzene, A new synthetic method of this compound is introduced below., Formula: C6H4BrCl

General procedure: To a mixture of aryl halide (0.3 mmol), NiCl2(H2O)1.5 [1] (0.0075 mmol, 2.5 mol percent), was charged dry THF (1 mL). The mixture was pumped and refilled with nitrogen for three times. The resulting mixture was stirred at -10 under nitrogen for 30 min. The reaction mixture was quenched through the addition of ice MeOH, then poured into a separatory funnel containing saturated aqueous NH4Cl (ca. 5 mL) and extracted with EtOAc (3 x 5 mL). The combined organic layers were washed with brine and dried over Na2SO4. The crude product was purified by column chromatography. Extent of isomerization can be easily determined via 1H NMR spectroscopy by comparison of the intergral of the singlet from the t-butyl group (1.3-1.4 ppm, 9H) to the integral of the doublet from the benzylic S3 protons of the i-butyl group (2.4-2.5 ppm, 2H). The doublet from the methyls of the i-butyl group could additionally be used (ca. 0.8 ppm, 6H).

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:
Article; Wu, Zhenghan; Si, Tengda; Xu, Guangqing; Xu, Bin; Tang, Wenjun; Chinese Chemical Letters; vol. 30; 3; (2019); p. 597 – 600;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 13918-92-8, 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. 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 4.00 g (21.4 mmol) C-3, 4.3 mL (32 mmol) 2,4-difluorobenzenesulfonyl chloride, 5.2 mL (64 mmol) pyridine and 50 mL DCM is stirred at RT for 5 h. After completion of the reaction, the solvent is removed under reduced pressure, the crude product is taken up in 50 mL water and extracted twice with 100 mL DCM. The combined organic layers are dried over MgSO4 and the solvent is removed under reduced pressure. The crude product can be used without further purification. Yield: 7.88 g (91%).

The chemical industry reduces the impact on the environment during synthesis 2,4-Difluorobenzene-1-sulfonyl chloride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; The designation of the inventor has not yet been filed; EP2546249; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application 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.

Production Example 1 Synthesis of dihydrate of Compound (I) Methanol (149 L), 7-hydroxy-1H-quinolin-2-one (14.87 kg), and potassium hydroxide (6.21 kg) were mixed in a reaction vessel, and the resulting mixture was stirred. After dissolution, 1-bromo-4-chlorobutane (47.46 kg) was added thereto, and the resulting mixture was stirred under reflux for seven hours. Thereafter, the mixture was stirred at 10 C. for one hour. The precipitated crystal was centrifuged and washed with methanol (15 L). The wet crystal was collected and placed in a tank. Water (149 L) was added thereto, followed by stirring at room temperature. After centrifugation, the result was washed with water (30 L). The wet crystal was collected and placed in a tank. After adding methanol (74 L), the mixture was stirred under reflux for one hour, cooled to 10 C., and then stirred. The precipitated crystal was centrifuged and washed with methanol (15 L). The separated crystal was dried at 60 C. to obtain 7-(4-chlorobutoxy)-1H-quinolin-2-one (15.07 kg).

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

Reference:
Patent; Sato, Tetsuya; Minowa, Takuya; Hoshika, Yusuke; Toyofuku, Hidekazu; US2015/86632; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

A common compound: 54932-72-8, name is 4-Bromo-1-chloro-2-methylbenzene, belongs to chlorides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 54932-72-8

Nitrogen gas was purged through a stirred solution of 5-bromo-2-chiorotoluene (452 muIota, 3.41 mmol) in 1 ,4-dioxane (15 ml) for 30 mins. 2,2′-Bis(diphenylphosphino)-1 , 1 ‘- binaphthyl (212 mg, 0.34 mmol), Pd(OAc)2 (153 mg, 0.68 mmol) and Cs2C03 (2.22 g, 6.81 mmol) were then added. The stirred solution was then purged of nitrogen for a further 30 min after which 1-Boc-3-aminopyrrolidine (745 muIota, 4.09 mmol) was added and solution stirred at reflux for 48 h under N2. The solvent was then evaporated in vacuo and the crude residue dissolved in EtOAc (40 ml) which was then washed with water (2 x 30 ml), brine (2 chi 30 ml), dried with Na2S04, filtered and concentrated. The crude residue was then purified by column chromatography (100% CyHex to 10% EtOAc/CyHex) to obtain WIN-321 -142-01 as a solid (111 mg, 10.4%).1H NMR (CDCI3): delta 7.13 (d, J 8.4 Hz, 1H), 6.48 (d, J 2.6 Hz, 1H), 6.39 (dd, J 8.58, 2.86 Hz, 1H), 3.99 (br. s., 1H), 3.79-3.57 (m, 2H), 3.56-3.38 (m, 2H), 3.31 -3.14 (m, 1H), 2.30 (s, 3H), 2.10 – 2.26 (m, 1 H), 1.96 – 1.79 (m, 1 H), 1.47 (s, 9H). MS, m/z = 255 (100) [M-56], 257 (30).

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, 54932-72-8, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE UNIVERSITY OF MELBOURNE; THE WALTER AND ELIZA HALL INSTITUTE OF MEDICAL RESEARCH; SLEEBS, Brad; PURCELL, Damian Francis John; JACOBSON, Jonathan; LEWIN, Sharon; NGUYEN, William; (163 pag.)WO2017/219083; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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 2533-69-9, Recommanded Product: 2533-69-9

(a) 2-Trichloromethyl-6-trifluoromethyl-1H-benzoimidazole. To a solution of 4-trifluoromethyl-benzene-1,2-diamine (1.76 g, 10 mmol, Lancaster) in DCM (20 mL) was added methyl 2,2,2-trichloroacetimidate (1.94 g, 11 mmol, Aldrich) and glacial acetic acid (3 mL) with stirring at room temperature. The reaction mixture was stirred at room temperature for 16 h and concentrated in vacuo. The residue was purified by silica gel column chromatography (35% EtOAc/hexane) to give the title compound as a brown solid. MS (ESI, pos. ion) m/z: 303 (M+1).

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

Reference:
Patent; Hulme, Christopher; Ncube, Mghele Vellah; Norman, Mark H.; Ognyanov, Vassil I.; Pettus, Liping H.; Wang, Xianghong; Zhu, Jiawang; US2005/165049; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, 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 94-97-3, Recommanded Product: 5-Chloro-1H-benzo[d][1,2,3]triazole

General procedure: A mixture of azole (0.2 mmol), ketone (0.3 mmol, 1.5equiv.), NaHCO3 (33.6 mg, 2.0 equiv.), I2 (101.6 mg, 2.0 equiv.), and 1,2-dichloroethane (2 mL) was stirred at 80 C for 24 h. After cooling to room temperature, the reaction mixture was quenched with a saturated solution of Na2S2O3 (5 mL) and extracted with ethyl acetate (3×5 mL). The combined organic phases were washed with brine (10 mL), dried over anhydrous magnesium sulfate, filtered, and concentrated. The residue was purified by flash column chromatograph, using a mixture of petroleum ether and ethyl acetate (5:1-2:1) as eluent to afford the corresponding products. The identity and purity of the products was confirmed by 1H and 13C NMR spectroscopic analysis.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Chen, Wenlin; Yan, Rulong; Tang, Dong; Guo, Shuaibo; Meng, Xu; Chen, Baohua; Tetrahedron; vol. 68; 38; (2012); p. 7956 – 7959;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 93765-83-4, 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. 93765-83-4, name is 1-Bromo-5-chloro-2-fluoro-4-methylbenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation 12To a solution of 1-bromo-5-chloro-2-fluoro-4-methylbenzene (Comm, 10 g, 44.7 mmol) in methanol (200 ml_) was added 1 ,1′-binaphthalene-2,2′-diylbis(diphenylphosphine) – dichloropalladium (1:1) (358 mg, 0.447 mmol) and N,N-diethylethanamine (8.11 ml_, 58.2 mmol). The resulting mixture was placed in a bomb and pressurized with carbon monoxide to 80 psi and heated at 80C for 18 hours. The reaction mixture was then concentrated in vacuo to yield a semi-solid, which was dissolved in EtOAc (300 ml_) and washed with water (200 mL). The organic layer was separated, dried over magnesium sulphate, filtered and concentrated in vacuo to yield an orange oil, which solidified on standing (9.87 g). The solid was purified by silica gel chromatography eluting with 0 to 20% EtOAc in heptane to afford the title compound as a crystalline white solid (8.47 g, 93%).1H NMR (400 MHz, CDCI3): delta 2.40 (s, 3H), 3.92 (s, 3H), 7.03 (d, 1 H), 7.91 (d, 1 H) LCMS Rt = 1 .64 minutes Molecular ion not observed

The synthetic route of 1-Bromo-5-chloro-2-fluoro-4-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; PFIZER LIMITED; BROWN, Alan, Daniel; RAWSON, David, James; STORER, Robert, Ian; SWAIN, Nigel, Alan; WO2012/7868; (2012); A2;,
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. 3972-56-3, name is 1-tert-Butyl-4-chlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C10H13Cl

20 parts of water,40 parts of acetone,And 20 parts of potassium carbonate were mixed,Three parts of raw material A are added. After stirring for 1 hour,10 parts of raw material B was charged, the temperature was raised to 50 ° C. while stirring,Stir for an additional 1 hour. after that,Concentrate using a rotary evaporator,And dried to obtain a dispersant.N – (4 – aminophenyl) acetamide was used as the raw material A of the dispersant preparation example,Using 1-tert-butyl-4-chlorobenzene as the raw material B,Dispersant 1 was obtained.

According to the analysis of related databases, 3972-56-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Dispersed materials Institute; Umemura, Kazuyuki; Ito, Shiho; Suzuki, Junji; Nishida, Atsushi; (15 pag.)JP2016/108519; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 60811-18-9,Some common heterocyclic compound, 60811-18-9, name is 4-Bromo-1-chloro-2-fluorobenzene, molecular formula is C6H3BrClF, 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. 4-chloro-3-fluorobenzoylpropionic acid To a solution of succinic anhydride (6.0 g) in tetrahydrofuran (60 ml) was added dropwise the Grignard prepared from 1.5 g (0.062 mole) of magnesium turnings and 10.5 g (0.05 mole) of 1-bromo-4-chloro-3-fluorobenzene using the procedure of part a. When the addition was completed, the resulting suspension was stirred for 2 hours at 45 C. after which water (100 ml) was added slowly and the resulting mixture was acidified with concentrated hydrochloric acid to pH=1. The ether layer was separated and extracted with 5% aqueous sodium hydroxide (3*100 ml). The combined aqueous solutions were washed with ether (1*100 ml). The combined basic aqueous layers were acidified with concentrated hydrochloric acid to pH 1 and extracted with ethyl acetate (3*150 ml). The combined organic extracts were washed with water (1*150 ml) and brine (1*150 ml), dried over anhydrous magnesium sulfate and evaporated in vacuo to give 7.1 g (62%) of the product as a yellow orange solid. The resulting acid was converted to the desired product using the procedure of Example 11d-e. Compound 83 was prepared following essentially the same procedure.

The synthetic route of 60811-18-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rohm and Haas Company; US5552409; (1996); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 118-69-4, name is 2,6-Dichlorotoluene, 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 118-69-4, SDS of cas: 118-69-4

Example 1 3-Chloro-2-methylphenol Process Variant a1 16.1 g (0.1 mol) of 2,6-dichlorotoluene and 19.8 g (0.3 mol) of potassium hydroxide (85%) are heated in 30 ml of diethylene glycol at a bath temperature of 190 C. for 18 hours. The water released by the reaction is distilled off. After cooling, the reaction mixture is stirred with 100 ml of water until a solution is obtained and extracted three times with 50 ml of dichloromethane. The aqueous phase is admixed with 35 ml of 30% hydrochloric acid and extracted three times with 70 ml of dichloromethane. The organic phases are dried over sodium sulphate and concentrated under reduced pressure. 3-Chloro-2-methylphenol is obtained as a solid (12.4 g, content by HPLC: 83%, 72% of theory). NMR (d6-DMSO): 6.75 (d, 1H, aromatic), 6.85 (d, 1H, aromatic) 7.0 (t, 1H, aromatic), 9.8 (s, 1H, phenolic OH)

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

Reference:
Patent; Huebsch, Walter; Lantzsch, Reinhard; Mueh, Thorsten; Weintritt, Holger; US2003/92944; (2003); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics