Month: February 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. 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

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. 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine

b) The 3-chloro-N-(tetrahydro-2H-pyran-4-yl)[1,2,4]triazolo[4,3-b]-pyridazin-6-amine can be prepared in the following way:2.1 cm3 of tetrahydro-2H-pyran-4-amine and 3 cm3 of triethylamine are added to a solution of 2 g of commercial 3,6-dichloro[1,2,4]triazolo[4,3-b]pyridazine in 20 cm3 of N,N-dimethylformamide. The reaction mixture is stirred at 20 C. for 18 h and 3 h at 50 C., and then cooled to 20 C., before the addition of 20 cm3 of water. The white precipitate is spin-filter-dried and then washed successively with water and ether. 1.3 g of 3-chloro-N-(tetrahydro-2H-pyran-4-yl)[1,2,4]triazolo[4,3-b]pyridazin-6-amine are thus obtained in the form of a white powder, the characteristics of which are as follows:MASS SPECTRUM: Waters ZQ: MH+m/z=254+; MH-=252-

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

Reference:
Patent; SANOFI; US2012/40987; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 1008361-80-5, A common heterocyclic compound, 1008361-80-5, name is 4-Bromo-3-chlorobenzene-1,2-diamine, molecular formula is C6H6BrClN2, 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.

3.40 g (approx. 14.700 mmol) of the compound from example 44A was dissolved in 200 ml ethanol and 2.39 g (19.865 mmol) /rans-2,3-dihydroxy-l,4-dioxane was added. It was stirred overnight at room temperature. The reaction mixture was concentrated by evaporation to 2/3, the product that crystallized out was filtered off, washed with a little ethanol and dried under high vacuum. We obtained 3.33 g (89% of theor.) of the target compound.LC-MS (method 4): R, = 1.04 min; MS (EIpos): m/z = 243 [M+H]+. 1H-NMR (400 MHz, DMSO-D6): delta [ppm] = 8.04 (d, IH), 8.19 (d, IH), 9.09 (d, IH), 9.10 (d, IH).

The synthetic route of 1008361-80-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; BAeRFACKER, Lars; KAST, Raimund; GRIEBENOW, Nils; MEIER, Heinrich; KOLKHOF, Peter; ALBRECHT-KUePPER, Barbara; NITSCHE, Adam; STASCH, Johannes-Peter; SCHNEIDER, Dirk; TEUSCH, Nicole; RUDOLPH, Joachim; WHELAN, James; BULLOCK, William; PLEASIC-WILLIAMS, Susan; WO2010/20363; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 87851-77-2, 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 87851-77-2 as follows.

EXAMPLE 4 Preparation of (E)-2-[1-(3-chloro-2-propenyloxyimino)propyl]-5-(1,3-dimethyl-1H-pyrazol-5-yl)cyclohexane-1,3-dione (Compound No. 4) STR19 To 10 ml of a solution of 5.60 g (21.3 mmols) of 5-(1,3-dimethyl-1H-pyrazol-5-yl)-2-propionylcyclohexane-1,3-dione in methanol was added 57 ml (21.7 mmols) of 0.38 mol ethanolic solution of (E)-3-chloro-2-propenyloxyamine. The mixture was reacted for 10 hours with stirring. After completion of the reaction, the reaction mixture was concentrated under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane:ethyl acetate=2:1) to give 6.84 g of the product. Physical properties: Melting point, 83¡ã-85¡ã C., Yield, 91.1percent. 1 H NMR (CDCl3, TMS), ppm. delta1.13 (3H, t, J=7 Hz) 2.16 (3H, s) 2.5-3.2 (6H, m) 3.2-3.7 (1H, m) 3.73 (3H, s) 4.51 (2H, d, J=6 Hz) 5.1 (1H, s) 5.9-6.5 (2H, m).

According to the analysis of related databases, 87851-77-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Nihon Nohyaku Co., Ltd.; US4863504; (1989); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics