Month: June 2021

Synthetic Route of 4584-46-7, The chemical industry reduces the impact on the environment during synthesis 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, I believe this compound will play a more active role in future production and life.

(1) 1.52 g (10 mmol) of methyl 4-hydroxybenzoate was dissolved in 40 ml of N,N-dimethylformamide and 2.16 g (15 mmol) of 2-dimethylaminoethyl chloride hydrochloride and 4.15 g (30 mmol) of potassium carbonate were further added. The mixture was heated at 80 C. and stirred overnight. After cooling, water was added to the reaction mixture, the obtained mixture was extracted twice with ethyl acetate, and the extract was washed with brine. The organic phase was dried (Na2 SO4) and the solvent was distilled off. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=70:1 to 15:1 (v/v)) to obtain 0.69 g (3.09 mmol) of methyl 4-(2-dimethylaminoethoxy)benzoate as a pale brown oily substance. Its spectroscopic data are as follows: 1 H-NMR (CDCl3) delta (ppm):2.34 (6H, s), 2.75 (2H, t, J=5.8 Hz), 3.88 (3H, s), 4.1 2 (2H, t, J=5.6 Hz), 6.93 (2H, d, J=9.2 Hz), 7.98 (2H, d, J=9.2 Hz)

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-Chloro-N,N-dimethylethanamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Terumo Kabushiki Kaisha; US6069149; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 53531-69-4, name is (4-Bromophenyl)methanesulfonyl chloride, 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 53531-69-4, COA of Formula: C7H6BrClO2S

To a stirred mixture of potassium carbonate (74.8 g, 0.542 mol) in DCM (70 mL) and H20 (220 mL) at -10C was added pyrrolidine (21.2 g, 0.298 mol) in portions, and the resulting mixture was stirred for 20 min. Then (4-bromophenyl)methanesulfonyl chloride(73.0 g, 0.271 mol) in DCM (400 mL)was added drop-wise. The resultant mixture was stirred for 1 h at RT. The organic phase was separated, washed with H20, brine, dried over Na2S04, and concentrated in vacuo. The residue was recrystallized from 5% EtO Ac/petroleum ether to give the title compound. 1H NMR (300 MHz, CDC13) delta: 7.52 (d, 2H), 7.25 (d, 2H), 4.20 (s, 2H), 3.20-3.30 (m, 4H), 1.80-1.92 (m, 4H).

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, (4-Bromophenyl)methanesulfonyl chloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME CORP.; CHILDERS, Matthew Lloyd; DINSMORE, Christopher; FULLER, Peter; GUERIN, David; KATZ, Jason David; PU, Qinglin; SCOTT, Mark E.; THOMPSON, Christopher F.; ZHANG, Hongjun; FALCONE, Danielle; TORRES, Luis; BRUBAKER, Jason; ZENG, Hongbo; CAI, Jiaqiang; DU, Xiaoxing; WANG, Chonggang; BAI, Yunfeng; KONG, Norman; LIU, Yumei; ZHENG, Zhixiang; WO2014/146490; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 39191-07-6, 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. 39191-07-6, name is 1-(3-Chlorophenyl)-N-methylmethanamine, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The procedure is as follows: 3 mg of catalyst CoPz (hmdtn) 4 is weighed into a quartz jacketed photoreactor, and then 25 mL of a reaction solvent, acetonitrile (abbreviated as CH3CN), is added. CoPz(hmdtn)4 was completely dissolved in CH3CN under stirring. Further, 0.01 mmol of the auxiliary 1,8-diazabicycloundec-7-ene (abbreviated as DBU) and 1 mmol of N-methylbenzylamine were added to the above system. Stirring was continued for 2 h in the dark. Then, at 1 atm oxygen and lambda ? 420 nm visible light (using a xenon lamp as a light source, a 420 nm filter is used to filter out light having a wavelength of less than 420 nm, The following examples are the same as the light intensity of 1.01 W·cm -2 ) for 3 h under light conditions. The reaction products were qualitatively analyzed and quantified by gas chromatography-mass spectrometry (GC-MS) and gas chromatography (GC). The experiment was recorded as Entry 1.

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

Reference:
Patent; South Central University for Nationalities; Yang Changjun; Jin Juanjuan; Deng Kejian; Zhang Bingguang; (12 pag.)CN108623494; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 72934-36-2, 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 72934-36-2 as follows.

Step 3: iPr2NEt (0.35 g) was added into the solution of methyl 4-(4-chloro-6-(2,2,2- trifluoroethoxy-D2)- 1,3,5 -triazin-2-ylamino)benzoate (1 g) and 1 -(4- chlorophenyl)cyclopropanamine (0.46 g) in THF (15 mL). The reaction was stirred at70C for 16 hours. Solvents were removed under vacuum to give a residue, to which 100 ml of EtOAc were added. The organic phase was washed with water (2 x 20 mL) and brine (15 mL), dried over Mg504 and concentrated under vacuum to give methyl 4-(4-(1- (4-chlorophenyl)cyclopropylamino)-6-(2,2,2-trifluoroethoxy-D2)- 1,3 ,5-triazin-2- ylamino)benzoate (1.30 g) which was used in the further reaction without purification.

According to the analysis of related databases, 72934-36-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WANG, Tao; YIN, Zhiwei; ZHANG, Zhongxing; SCOLA, Paul Michael; WO2014/116766; (2014); 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. 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. Formula: C7H6Cl2

Sub-step 1.1: In a 3000mL three-necked flask, add solid sodium methoxide 450g and dimethyl sulfoxide 700g, stir and heat up to 180 , start dropwise addition of 2,6-dichlorotoluene 1000g, after 4h dropwise addition, keep the reaction 2 hours, transfer to a distillation flask, distill dimethyl sulfoxide under reduced pressure through a rectification column (applied in the next batch), and distill under reduced pressure for 5 hours at a temperature of 130 C and a pressure of -0.095MPa.Distilled substrate.Substep 1.2: Transfer the distillation substrate to a three-necked flask, add 80g of dimethyl sulfate dropwise at 80 C, complete the dropwise addition within 2h, hold the reaction for 1.5 hours, add 1500g of water, and after washing, transfer the oil layer to the distillation flask. Distillation under reduced pressure for 8 hours at a temperature of 120 C and a pressure of -0.095MPa,906.1g of 2-methyl-3-chloroanisole was obtained.

The synthetic route of 118-69-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Xi’an Zhengyang Jiahe Chemical Technology Co., Ltd.; Guo Xiangxiang; (8 pag.)CN111018693; (2020); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 93765-83-4, The chemical industry reduces the impact on the environment during synthesis 93765-83-4, name is 1-Bromo-5-chloro-2-fluoro-4-methylbenzene, I believe this compound will play a more active role in future production and life.

A mixture of 1-bromo-5-chloro-2-fluoro-4-methylbenzene (5.0 g, 23 mmol), copper(I) cyanide (4.0 g, 45 mmol) and copper(I) iodide (8.6 g, 45 mmol) in NMP (50 mL) was heated at 140C over night. After cooling to room temperature, the mixture was filterted and the filtrate was diluted with water (100 mL) and extracted with ethyl acetate (100 mL chi 3). The combined organic layers were washed with water (100 mL) and dried over Na2SO4. The solvent was removed and the residue was purified by SGC (eluting with petroleum ether/EtOAc = 10/1) to afford 5-chloro-2-fluoro-4-methylbenzonitrile (1.7 g, 45% yield) as a white solid

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-5-chloro-2-fluoro-4-methylbenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; GENENTECH, INC.; XENON PHARMACEUTICALS INC.; CHEN, Chien-An; CHOWDHURY, Sultan; DEHNHARDT, Christoph Martin; SUN, Shaoyi; WO2014/144545; (2014); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 1435-44-5, A common heterocyclic compound, 1435-44-5, name is 1-Chloro-2,4-difluorobenzene, molecular formula is C6H3ClF2, 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.

1-Chloro-2,4-difluoro-5-nitrobenzene. To a stirred solution of 1-chloro-2,4-difluorobenzene (0.829 g, 5.58 mmol) in concd H2 SO4 (8.0 mL) at 0 C., KNO3 (0.565 g, 5.59 mmol) was added in one portion. The resulting solution was allowed to warm to room temperature and stirred overnight at room temperature. It was then poured into ice (80 g) and extracted with ethyl acetate (75 mL). The ethyl acetate was dried over anhydrous Na2 SO4, removed under vacuum, and the resulting oil was dried further under vacuum to afford 1.007 g (93%) pure (1 H NMR) title compound as a light red oil; 1 H NMR (CDCl3) delta7.17 (dd, 1H, J1 =9.9 Hz, J2 =8.4 Hz), 8.24 (t, 1H, J=7.5 Hz).

The synthetic route of 1435-44-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; State of Oregon, acting by and through the Oregon State Board of Higher Education, acting for and on behalf of the Oregon Health Sciences University and the University of Oregon, Eugene Oregon; Acea Pharmaceuticals, Inc.; The Regents of the University of California; US5631373; (1997); 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. 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, A new synthetic method of this compound is introduced below., Product Details of 1996-29-8

A 3L 3-neck round bottom flask equipped with a mechanical stirrer, a temperature controller, and a nitrogen inlet was charged with potassium tert-butoxide (Aldrich 95%, 84.6 g, 0.716 mol) and DMSO (400 mL, 4×) at room temperature and stirred for 15 minutes. To this solution was added pyrazole 2 (59 g, 0.719 mol) followed by a DMSO rinse (50 mL, 0.5×). The resulting orange turbid solution was stirred for 15 minutes and fluoride 1 (100 g, 0.477 mol) was added followed by a DMSO rinse (50 mL, 0.5×). This mixture was then heated to 50 C. and held for 5 hours at this temperature. After cooling to room temperature, the reaction mixture was diluted with MTBE (750 mL), and water (500 mL) was added to give a brown turbid mixture. After 15 minutes stirring, the organic layer was separated and sequentially washed with 1 N HCl (250 mL), brine (250 mL), and water (250 mL). Solution assay of organic layer was carried out using GC (conversion >99%, solution yields of 3 and its regioisomer 4 were 83% and 17%, respectively). The MTBE solution was then concentrated under vacuum to a total volume of about 200 mL (KF showed 0.737% water). THF (500 mL) was added, and concentrated to 2× solution (KF=0.158%). THF addition-concentration sequence was repeated to give a 2× solution (KF=0.023%), which used directly in the next step.Analytical samples of compounds 3 and 4 were purified by column chromatography and characterized: Compound 3: white crystals; M.p.: 76 C. (DSC onset temperature). 1H NMR (400 MHz, CDCl3) delta 7.80 (1H, d, J=2.3 Hz), 7.61 (1H, d, J=8.6 Hz), 7.58 (1H, d, J=2.5 Hz), 7.22 (1H, dd, J=8.6, 2.6 Hz), 6.27 (1H, d, J=2.5 Hz), 2.38 (3H, s); 13C NMR (100 MHz, CDCl3) delta 150.8, 140.6, 134.6, 134.1, 132.0, 129.0, 128.2, 115.4, 107.0, 13.6. Compound 4: white crystals; 1H NMR (400 MHz, CDCl3) delta 7.65 (1H, d, J=8.6 Hz), 7.62 (1H, d, J=1.5 Hz), 7.43 (1H, d, J=2.5 Hz), 7.35 (1H, dd, J=8.6, 2.2 Hz), 6.21 (1H, s), 2.19 (3H, s); 13C NMR (100 MHz, CDCl3) delta 140.6, 140.2, 140.0, 134.1, 133.9, 130.8, 130.2, 120.7, 105.9, 11.4.

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; Bednarz, Mark S.; Burgoon, JR., Hugh Alfred; Iimura, Shinya; Kanamarlapudi, Ramanaiah C.; Song, Qiuling; Wu, Wenxue; Yan, Jie; Zhang, Haiming; US2009/62540; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 13526-66-4, 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 13526-66-4 as follows.

Synthesis of intermediate IV-02IV-01 IV-02To a solution of 3-bromo-6-chIoroimidazo[1 ,2-b]pyridazine (IV-01) (450 mg, 1.936 mmol) in 1 ,4-dioxane (8 mL) was added 3-(N-Boc-aminomethyl)pyridine-5- boronic acid pinacol ester (679 mg, 2.033 mmol), aq. Na2C03 2 (3 mL, 6 mmol) and PdCI2(PPh3)2 (136 mg, 0.194 mmol). The resulting mixture was heated at 80 C in a sealed tube for 8 h. On cooling, the mixture was diluted with DC and water. Layers were separated and the aqueous phase was extracted twice with DCM. The combined organic extracts were dried (Na2S04), filtered and concentrated. The residue was purified by flash chromatography (Biotage) using MeOH:DCM 0:100 to 20:80 as eluent to afford intermediate IV-02 (525mg, 75%).

According to the analysis of related databases, 13526-66-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CENTRO NACIONAL DE INVESTIGACIONES ONCOLOGICAS (CNIO); PASTOR FERNANDEZ, Joaquin; ALVAREZ ESCOBAR, Rosa Maria; RIESCO FAGUNDO, Rosario Concepcion; GARCIA GARCIA, Ana Belen; RODRIGUEZ HERGUETA, Antonio; MARTIN HERNANDO, Jose Ignacio; BLANCO APARICIO, Carmen; CEBRIAN MUNOZ, David Alvaro; WO2012/156756; (2012); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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. SDS of cas: 2533-69-9

A solution of aniline of preparation 28 (79 mg, 0.56 mmol) in acetic acid (3 ml) was treated with methyl-2,2,2-trichloroacetimidate (77 mul, 0.62 mmol) and the resulting solution was left to stir at room temperature for 16 hours. Water (10 ml) was added and the reaction stirred for a further hour. The precipitate was filtered off and dried in vacuo. The resulting solid was suspended in a mixture of acetonitrile and water (3:1 by volume, 4 ml) and treated with a solution of (3aR,6aS)-2-methyloctahydropyrrolo[3,4-c]pyrrole (148 mg, 1.17 mmol) in a mixture of acetonitrile (0.75 ml) and water (0.25 ml). After 3 hours the solvent was removed in vacuo and the residue dissolved in dichloromethane (15 ml), washed with saturated sodium bicarbonate (2*15 ml), dried (sodium sulfate) and concentrated in vacuo. Purification by flash column chromatography on silica gel eluding with dichloromethane:methanol:880 ammonia (99:1:0.1 changing to 93:7:0.7, by volume) gave the title compound as a colourless solid (133 mg). 1H NMR (400 MHz, CD3OD): delta 7.19 (1H, s), 6.87-6.84 (1H, d), 4.39-4.27 (2H, m), 3.90-3.84 (1H, m), 3.75-3.71 (1H, m), 3.09-2.95 (2H, m), 2.79-2.72 (2H, m), 2.51-2.40 (2H, m), 2.46 (3H, s), 2.33 (3H, s) ppm. MS (APCI): m/z 303 [M+H]+, 301 [M-H]-

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

Reference:
Patent; Lane, Charlotte Alice Louise; Price, David Anthony; US2006/111416; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics