Author: Jessica.F

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. 627-42-9, name is 2-Methoxyethyl chloride, A new synthetic method of this compound is introduced below., SDS of cas: 627-42-9

Starting Material Synthetic Example 106 4-Hydroxybenzaldehyde (300 g) and 2-chloroethyl methyl ether (279 g) were dissolved in DMF (3 L) and potassium carbonate (408 g) was added. The mixture was stirred with heating at 60 C. for 16 hr. After the reaction, the reaction mixture was poured into water and liberated oil was extracted with ethyl acetate. The organic layer was washed with 1N aqueous sodium hydroxide solution and washed with saturated brine. The organic layer was dried over anhydrous magnesium sulfate. After drying, the residue was concentrated under reduced pressure to give 4-(2-methoxyethoxy)benzaldehyde as an oil (212 g). 1H-NMR 270 MHz (CDCl3, ppm) delta: 9.87(1H, s), 7.82(2H, d), 7.02(2H, d), 4.18(2H, m), 3.77(2H, m), 3.44(3H, s).

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; Welfide Corporation; US6288061; (2001); B1;,
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. 6579-54-0, name is 2,6-Dichlorobenzenesulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 6579-54-0

General procedure: Benzenesulfonyl chloride (1 mmol) in butanone (5 mL) was heated with stirring to 40C, and cyanamide solution (50%)was added dropwise, then the temperature was raised to 60C and stirring continued for 3 h. The compound 7 (0. 8 mmol)was added and heated to 80C for 3 h. After cooling to 40C, the reaction mixture was poured into cold water while stirring, white crystals or powders were precipitated, filtered,washed with water, and dried. Analytically pure samples were obtained by recrystallization from aqueous ethanol.

According to the analysis of related databases, 6579-54-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Li, Jie; Zheng, Tu-Cai; Jin, Yi; Xu, Jian-Guo; Yu, Jian-Gang; Lv, Yan-Wen; Chemical and Pharmaceutical Bulletin; vol. 66; 1; (2018); p. 55 – 60;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

2268-05-5, name is 2,6-Dichlorofluorobenzene, 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. name: 2,6-Dichlorofluorobenzene

n a 250 ml four-necked flask, 64 g of 98% concentrated sulfuric acid was charged(0.606 mol) of 2,6-dichlorofluorobenzene was added dropwise to a stirred solution of 33 g of 98% concentrated sulfuric acid at 20 to 25 CMixed with 39 g of 98% concentrated nitric acid, 2.5 hThe addition is complete.After warming up to 40 ~ 45 C and heat 1.5 hours. After the end of the washing, to neutral, organic subtractionPressure dehydration after use.In a 250 ml four-necked flask285gSulfolane and87g (1.5mol) KF, after dehydration by adding the last step nitration products,In 195 ¡À 5 C heat 5h, vacuum distillation of the solvent and then distillation 2,3,4-trifluoronitrobenzene 91. 7g,The content was 99.8% and the yield was 85.5%

The synthetic route of 2268-05-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Binhai Yongtai Medical Chemical Co Ltd; He, Renbao; Shao, Hongming; (8 pag.)CN102249881; (2016); B;,
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. 95-81-8, name is 2-Chloro-5-methylaniline, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

(A-82-21) tert-Butyl 4-(2-chloro-5-methylphenylcarbamoyl)-3-[4-cyclopropyl-5-(3-isobutylcyclobutyl)isoxazol-3-yl]butanoate Mono-tert-butyl 3-[4-cyclopropyl-5-(3-isobutylcyclobutyl)isoxazol-3-yl]glutarate (2.83 g) and DMF (28 mL) were mixed. After an addition of 2-chloro-5-methylphenylamine (1.184 g), HOBt.H2O (1.28 g) and WSC.HCl (1.60 g) to the resultant solution, the mixture was stirred at RT for 2 days. To the reaction mixture was added saturated aqueous sodium bicarbonate, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate, water and brine, then dried over sodium sulfate. The sodium sulfate was filtered off and the filtrate was concentrated in vacuo. The resultant residue was purified by silica gel column chromatography (Eluent: ethyl acetate/hexane=1/15?1/10?1/8) to give the title compound (1.241 g).

The synthetic route of 95-81-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JAPAN TOBACCO INC.; US2012/322837; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 95-49-8, 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 95-49-8 as follows.

A 100 mL four-necked flask was charged with 47 mL (50 g) o-chlorotoluene, 0.25 g [BMIM]Cl-2AlCl3 was added, The ionic liquid is stirred to disperse evenly. And then into the system 20 mL / min by concentrated sulfuric acid drying of chlorine, Reaction at 30 C for 12 h to give dichlorotoluene, The tail gas is removed by NaOH solution to remove unreacted Cl2.

According to the analysis of related databases, 95-49-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NANJING ZHONGTENG CHEMICAL CO LTD; JIANGSU ZHONGTENG CHEMICAL CO LTD; Zhong, Hua; Lu, Minshan; Chen, Xiuzhen; Liu, Qiaobao; (7 pag.)CN104803827; (2016); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, 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 1996-29-8, name: 1-Bromo-4-chloro-2-fluorobenzene

1-bromo-4-chloro-2-fluorobenzene (5 g, 23.9 mmol, 1 equiv), piperazine-1 carboxylic acid tert- butyl ester (5.3 g, 1.15 eq), tris dibenzylideneacetone dipalladium (O) ( 0.43 g, 0.05 equiv), rac-BINAP (0.89g, 0.15 eq), sodium tert- butoxide (3.2 g, 1.4 eq) was slurried in toluene (60 mL), and heated overnight the mixture at 65 C.. After cooling to room temperature, it was added ethyl acetate (100mL). The black precipitate was removed by filtration. The filtrate was washed twice with 3N potassium carbonate solution. The organic phase was dried over sodium sulfate, concentrated and treated with 4NHCl in dioxane. The solid was collected by filtration, washed with ether, and dried under high vacuum 1- (4-chloro-2-fluorophenyl) piperazine was obtained as a dihydrochloride salt.

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-chloro-2-fluorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CHEMOCENTRYX INCORPORATED; ZHANG, PENGLIE; ZENG, YIBIN; (41 pag.)JP5654467; (2015); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 4090-55-5, These common heterocyclic compound, 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, 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.

The NCS was synthesized according to the literature (Kang and Li 2004). In a 250mL three-necked round-bottomed ask equipped with a magnetic stirrer and a reux condenser, PCL 18.40g (0.10mol) and acetonitrile (100mL) were mixed at 65C. Then, potassium thiocyanate 24.20g (0.25mol) was feed into the ask by batch addition, and the mixture was stirred at 65C for 8h. After the reaction, mixture was cooled slowly to room temperature, ltered, and evaporated under vacuum. A red mixture was obtained and washed with dichloromethane (30mL) to remove residual sylvite, ltered, and evaporated under vacuum. Repeat the post-processing process twice, an orange-red oily liquid was collected, and which was named as NCS, and the yield was 95%.

Statistics shows that 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide is playing an increasingly important role. we look forward to future research findings about 4090-55-5.

Reference:
Article; You, Ge-Yun; He, Hong-Wu; Feng, Bin; Tang, Yu-Ying; Cheng, Zhi-Quan; Fan, Fang-Fang; Chemical Papers; vol. 74; 8; (2020); p. 2403 – 2414;,
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. 2845-89-8, name is 1-Chloro-3-methoxybenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C7H7ClO

General procedure: Under N2 atmosphere, KOtBu (114.0 mg, 1.0 mmol), NHC-Pd(II)-Im complex 1 (5.2 mg, 1.0 mol %), dry toluene (1.0 mL), chlorobenzene 2a (0.8 mmol), and aniline 3a (0.96 mmol) were successively added into a Schlenk reaction tube. The reaction mixture was stirred under reflux for 4 h. Then the solvent was removed under reduced pressure and the residue was purified by a flash chromatography on silica gel to give the pure product 4a.

The synthetic route of 2845-89-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhu, Lei; Ye, Yue-Mei; Shao, Li-Xiong; Tetrahedron; vol. 68; 10; (2012); p. 2414 – 2420;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 33050-38-3, These common heterocyclic compound, 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-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.

c) The 3-chloro-6-(4-fluorophenyl)-1,2,4-triazolo[4,3-b]pyridazine can be prepared in the following way:a mixture of 4.16 g of 4-fluorophenylboronic acid, 9.37 g of barium hydroxide octahydrate, 2.20 g of [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) in a complex with dichloromethane (1:1) and 5.1 g of commercial 3,6-dichloro[1,2,4]triazolo[4,3-b]pyridazine in 40 cm3 of N,N-dimethylformamide containing 10 cm3 of water is heated in a bath at 80 C. for 1.5 1H). The beigey-brown suspension obtained is cooled to 20 C. and then poured into approximately 200 cm3 of water. The insoluble material is spin-filter-dried and washed successively with water and with ether, and then dried under vacuum at 20 C. The resulting beige solid is made into a paste in dichloromethane, spin-filter-dried, and dried under vacuum at 20 C. 1.24 g of 3-chloro-6-(4-fluorophenyl)-1,2,4-triazolo[4,3-b]pyridazine are thus obtained. 30 g of silica are added to the combined mother liquors and the mixture is evaporated to dryness under vacuum. This residue is deposited onto a bed of 10 g of silica in a sintered glass filter and elution is carried out with dichloromethane. An additional 1.60 g of 3-chloro-6-(4-fluorophenyl)-1,2,4-triazolo[4,3-b]pyridazine are thus recovered.

The synthetic route of 33050-38-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; sanofi-aventis; US2010/298315; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 39191-07-6, The chemical industry reduces the impact on the environment during synthesis 39191-07-6, name is 1-(3-Chlorophenyl)-N-methylmethanamine, I believe this compound will play a more active role in future production and life.

Following the procedure of Example 74 using 5,5-Dioxo-2-(4-nitrobenzoxy-carbonylamino)dibenzothiophene (Example 24) and the appropriate amine the following compounds were prepared.

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-(3-Chlorophenyl)-N-methylmethanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Block, Michael Howard; Donald, Craig Samuel; Brittain, David Robert; Foote, Kevin Michael; US2003/225097; (2003); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics