Tag: M.W=100-200

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;,
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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,
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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;,
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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;,
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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;,
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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;,
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Application of 106-39-8, The chemical industry reduces the impact on the environment during synthesis 106-39-8, name is 1-Bromo-4-chlorobenzene, I believe this compound will play a more active role in future production and life.

General procedure: A magnetic stirring bar, nanocrystalline CuO (10 mg, 3 mol %), KOH (112 mg, 2 mmol) and phenol/substituted phenol/ thiophenol (1.2 mmol) were added into an oven-dried flask (25 mL). The flask was sealed with a septum, followed by three cycles of evacuation and filling with dry nitrogen. Then aryl halide (1 mmol) and N,N-dimethyl acetamide (DMAc) (4 mL) were injected through a syringe. The flask was sealed and stirred under nitrogen until the completion of the reaction (as monitored by TLC or GC). The catalyst was recovered from the reaction mixture and washed several times with ethyl acetate. The catalyst-free reaction mixture was quenched with brine solution and the product was extracted with ethyl acetate. The combined organic extracts were dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated and the residue was purified by column chromatography on silica gel (hexane/ethyl acetate, 80/20) to afford the product with high purity.

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

Reference:
Article; Babu, S. Ganesh; Karvembu; Tetrahedron Letters; vol. 54; 13; (2013); p. 1677 – 1680;,
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Synthetic Route of 104-11-0, A common heterocyclic compound, 104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, molecular formula is C8H10ClN, 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.

PREPARATION EXAMPLE 8 Preparation of 1-(4-chlorobenzyl)-1,3-dimethyl-3-[2-methyl-1-(4-trifluoromethyl-pyrimidin-5-yl)-propyl]-urea (compound No. 1-532 of the present invention) 0.16g (1.0 mmol) of (4-chlorobenzyl)-methylamine was dissolved in 30 ml of pyridine, and 0.3g (1.0 mmol) of N-methyl-N-[2-methyl-1-(4-trifluoromethyl-pyrimidin-5-yl)-propyl]-carbamoyl chloride was dropwise added, followed by stirring at room temperature for 10 hours. To the reaction solution, 50 ml of water was added, followed by extraction with diethyl ether. The obtained organic phase was washed twice with 30 ml of a dilute citric acid aqueous solution, followed by drying over anhydrous magnesium sulfate. Diethyl ether was distilled off under reduced pressure, and the obtained crude product was purified by silica gel chromatography (developing solvent/n-hexane:ethyl acetate=8:1 to 3:1) to obtain0.22g (yield: 52%) of 1-(4-chlorobenzyl)-1,3-dimethyl-3-[2-methyl-1-(4-trifluoromethyl-pyrimidin-5-yl)-propyl]-urea as colorless crystals (melting point: 95-98C).

The synthetic route of 104-11-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KUMIAI CHEMICAL INDUSTRY CO., LTD.; IHARA CHEMICAL INDUSTRY CO., LTD.; EP1211246; (2002); 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. 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene, A new synthetic method of this compound is introduced below., Safety of 2,4-Dichloro-1-fluorobenzene

2,4-dichlorofluorobenzene 165g (1mol) and Catalyst Cat.1 0.77g were added to the reaction flask.Warm up to 40 C,Further introducing CO2 to 2 MPa, and stirring the reaction for 3 hours to obtain a reaction liquid;Further, 15.4 g (0.1 mol) of CCl4 was added dropwise to the reaction liquid, and the temperature was raised to 60 C.Insulation reaction for 2 hours,The hydrogen chloride formed by the reaction is absorbed by the falling film, and after the reaction is completed,The material obtained by the reaction is filtered to recover Catalyst Cat.1, and the filtrate is distilled under reduced pressure.2,4-dichloro-5-fluorobenzoyl chloride 44.95g,The yield was 98.8%.

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; Zhejiang Ben Li Technology Co., Ltd.; Gu Haining; Wu Zhengjie; Yu Yongzhi; Xu Hongshun; (10 pag.)CN109553524; (2019); A;,
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, Product Details of 2533-69-9

Put the compound (1,2-phenylenediamine) (2 g, 10 mmol) shown in Formula 3 at room temperature,Add acetic acid (20mL) to the reaction flask, cool in an ice bath, and slowly add the compound shown in Formula 1 (2,2,2-trichloroimino to methyl acetate) (1.3mL, 10mmol) as the starting material.After the addition was complete, the mixture was stirred at room temperature for 1 hour. TLC showed that the reaction was complete.Saturated sodium bicarbonate solution neutralized excess acid, extracted with ethyl acetate,Dry over anhydrous sodium sulfate, filter,Concentration gave the compound (2-trichloromethyl-benzopyrimidine) represented by Formula 3 (2.6 g, 60%).

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; Sun Yat-sen University; Fu Jiasheng; Lu Paxiama; G .leikexima Leidi; Hu Wenhao; Wang Xin; Huang Jiawu; Lin Zebin; (22 pag.)CN110606850; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics