Category: chlorides-buliding-blocks

Related Products of 85462-59-5,Some common heterocyclic compound, 85462-59-5, name is 2-Bromo-5-chloro-4-fluoroaniline, molecular formula is C6H4BrClFN, 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.

Step 2: 2-bromo-5-chloro-4-fluoro-N,N-dimethylaniline 2-Bromo-5-chloro-4-fluoroaniline (2.25 g, 0.01 mol), 40% formaldehyde solution (10 mL, 0.133 mol), and formic acid (4.6 g, 0.1 mol) were reacted at 100C for 3 hours. NaOH was added to adjust it to strongly alkaline, and then the resultant was extracted with CH2Cl2. The extract was dried, spin evaporated, and purified by silica gel column chromatography to give 2-bromo-5-chloro-4-fluoro-N,N-dimethylaniline (2.46 g, 97% yield). 1H-NMR (400 MHz, CDCl3):delta= 7.368 (d, J = 8.4 Hz, 1H), 7.079 (d, J = 6.8 Hz, 1H), 2.748 (s, 6H). MS m/z [ESI]: 253.9 [M+1].

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Bromo-5-chloro-4-fluoroaniline, its application will become more common.

Reference:
Patent; Chia Tai Tianqing Pharmaceutical Group Co.,Ltd; Centaurus BioPharma Co., Ltd.; Lianyungang Runzhong Pharmaceutical Co., Ltd.; XIAO, Dengming; XU, Xinhe; LIU, Xijie; HU, Yuandong; YU, Honghao; LIU, Zhihua; PENG, Yong; SUN, Yinghui; LUO, Hong; KONG, Fansheng; HAN, Yongxin; SUN, Jian; EP2952510; (2015); A1;,
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Related Products of 20850-43-5, These common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, 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.

General procedure: A mixture of the required pyrrole-2-carboxylic acid ethylester 9-12 (3 mmol), sodium hydride (4.5 mmol) and theappropriate arylmethylchloride (4.5 mmol) in dry dimethylformamide(5 mL) was stirred at room temperature for 48hours; after this time water was added and the resultingcrude material was extracted with diethyl ether (3 50 mL).The combined organic layers were dried over anhydroussodium sulphate, filtered, and concentrated under reducedpressure; the obtained residue was purified by means of flashchromatography using a mixture of ethyl acetate/cyclohexane (2:8, v:v) as eluent. Oil compounds 19 and 20 (yield: 55 and 53%, respectively) were immediately usedwithout further purification for the next step. Using this procedure,the following compounds were obtained:

Statistics shows that 5-(Chloromethyl)benzo[d][1,3]dioxole is playing an increasingly important role. we look forward to future research findings about 20850-43-5.

Reference:
Article; Salerno, Loredana; Modica, Maria N.; Romeo, Giuseppe; Pittala, Valeria; Cagnotto, Alfredo; Siracusa, Maria A.; Medicinal Chemistry; vol. 11; 2; (2015); p. 109 – 117;,
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Adding a certain compound to certain chemical reactions, such as: 622-86-6, name is (2-Chloroethoxy)benzene, 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 622-86-6, Formula: C8H9ClO

2-(3-bromophenyl)aceticacid (4.0 g, 18.6mmol) was dissolved in trifluoroacetic anhydride (3.6 mL), then (2-chloroethoxy)benzene(2.56 mL, 19.5 mmol) was added dropwise. The resulting mixture was allowed tostir at room temperature for overnight. The reaction mixture was quenched with saturatedaqueous sodium bicarbonate and then extracted twice with ethyl acetate. Theorganic phases were combined and dried over anhydrous magnesium sulfate andconcentrated on a rotary evaporator. Purification with normal phasechromatography (ethyl acetate/hexane) afforded 5.46 g (83%) of the desiredproduct as a yellow solid (83%). 1H NMR (400MHz, CDCl3) delta 8.07 (d, J =8.9 Hz, 2H), 7.47-7.40(m, 2H), 7.25-7.24 (m, 2H), 7.07(d, J = 8.9 Hz, 2H), 4.35 (m, 4H), 3.92-3.89(m, 2H); MS (ESI) (m/z) 353.0/355.0 (M+H)+.

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

Reference:
Article; Childers, Wayne; Fan, Rong; Martinez, Rogelio; Colussi, Dennis J.; Melenski, Edward; Liu, Yuxiao; Gordon, John; Abou-Gharbia, Magid; Jacobson, Marlene A.; Bioorganic and Medicinal Chemistry Letters; vol. 30; 2; (2020);,
Chloride – Wikipedia,
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Related Products of 1435-50-3, 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 1435-50-3 as follows.

Reference Example 76 1-(2,5-dichlorophenyl)-6-methoxyindan-1-ol To a solution of 1-bromo-2,5-dichlorobenzene (4.18 g, 18.5 mmol) in THF (25 mL) was added dropwise 1.6 M n-butyllithium hexane solution (13.8 mL, 22.1 mmol) at -78C, and the mixture was stirred for 30 min. Then, a solution of 6-methoxyindan-1-one (2.00 g, 12.3 mmol) in THF (15 mL) was added dropwise, and the mixture was stirred for 1 hr. To the reaction mixture was added saturated aqueous ammonium chloride solution and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound (1.95 g, yield 51%) as an oil. 1H-NMR (CDCl3) delta: 2.29 – 2.42 (1H, m), 2.52 (1H, s), 2.79 – 3.00 (2H, m), 3.04 – 3.23 (1H, m), 3.73 (3H, s), 6.53 (1H, d, J = 2.4 Hz), 6.87 (1H, dd, J = 8.3, 2.4 Hz), 7.16 – 7.30 (3H, m), 7.70 (1H, d, J = 2.3 Hz).

According to the analysis of related databases, 1435-50-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP2298731; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 14862-52-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 14862-52-3 name is 3,5-Dibromochlorobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Preparation of compound 7-1 After dissolving 1,3-dibromo-5-chlorobenzene (20 g, 73.98 mmol), phenyl boronic acid (22 g, 177.55 mmol), and Pd(PPh3)4(4.3 g, 3.699 mmol) in a mixture solvent of 2 M K3PO4aqueous solution 100 mL, toluene 400 mL, and 1,4-dioxane 100 mL in a flask, the mixture was stirred under reflux at 120C for 5 hours. After completing the reaction, an organic layer was extracted with ethyl acetate, and the remaining moisture was removed using magnesium sulfate. The residue was dried and separated with column chromatography to obtain compound 7-1 (23 g, 70%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Dibromochlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; ROHM AND HAAS ELECTRONIC MATERIALS KOREA LTD.; KANG, Hee-Ryong; KANG, Hyun-Ju; HONG, Jin-Ri; MOON, Doo-Hyeon; LIM, Young-Mook; KIM, Bitnari; KIM, Nam-Kyun; WO2015/178731; (2015); A1;,
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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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C6H3BrCl2

Example 2; Step 1; Magnesium turnings (5.38 g) and THF (50 ml) were placed in a dry flask equipped with a dropping funnel which contained a mixture of 1-bromo-3,5-dichiorobenzene (50 g) and THF (300 ml). 30 Milliliters of the solution in the dropping funnel was added to the flask. A few drops of dibromoethane were added to he flask to help initiate the reaction. After a few minutes, solvent in the reaction flask started to boil. The remaining solution in the dropping funnel was added drop wise. Ice water was used occasionally to coo. the reaction mixture. After the addition, the mixture was stirred at room temperature for two hours. Benzonitriie (22,82 g) was added to the reaction mixture. The mixture was refiuxed for 2 days. 3 N HC1 (300 mL} was added, The mixture was stirred for 4 hours and extracted using ethyl acetate. The organic layer was collected in a separatory funnel and concentrated. The obtained oil (49 g) was used in the next step without further purification.

The synthetic route of 19752-55-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TRANSITIONS OPTICAL, INC.; WO2012/82506; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 7149-75-9, 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 7149-75-9 as follows.

In a 150 mL Schlenk tube equipped with a stirring bar, 5.79 g (22.0 mmol) of 4-bromodibenzothiophene represented by the above chemical formula (99), 4-chloro-3- 3.74 g (26.4 mmol) of methylaniline, 3.70 g (33.0 mmol) of potassium-tert-butoxide, 99 mg (0.44 mmol) of palladium (II) acetate and 60 mL of dehydrated toluene were placed and degassed and then tri- Butyl phosphine (267 mg, 1.32 mmol), and the mixture was sealed and stirred at 100 ° C. for 10 hours.After cooling to room temperature, the reaction mixture was poured into water, extracted with methylene chloride, and washed with water. After drying the organic layer with anhydrous sodium sulfate, the solvent was distilled off. The obtained crude product was purified by silica gel column chromatography using hexane: methylene chloride (4: 1) as an eluent.By carrying out the above steps, a compound represented by the above chemical formula (109) was obtained in a yield of 3.75 g in a yield of 53percent. Identification of the compound was carried out by mass spectrometry where the molecular ion peak matched with the object.

According to the analysis of related databases, 7149-75-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NIPPON HOSO KYOKAI <NHK>; KANTO CHEM CO INC; FUKAGAWA HIROHIKO; SHIMIZU TAKAHISA; TAKAHASHI JUNPEI; SHINNAI SATONOBU; TSUCHIYA KAZUHIKO; (53 pag.)JP2015/160849; (2015); A;,
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Chlorides – an overview | ScienceDirect Topics

Related Products 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.

General procedure: 3-Hydroxybenzaldehyde (20 mmol) and the corresponding N-methylbenzylamine (8 mmol) were dissolved in methanol (5 mL). Acetic acid (0.4 mL) and sodium cyanoborohydride (16 mmol) were added and the mixture was stirred for 18 h at room temperature. The solvent was evaporated, the residue was suspended in satd. Na2CO3 solution(100 mL), and extracted with dichloromethane (3 x 50 mL). The combined organic layers were dried over sodium sulfate and evaporated. The residue was purified by flash column chromatography (1:1 hexane/ethyl acetate with 2 % N-ethyl-N,N-dimethylamine).

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

Reference:
Article; Wolfgardt, Annette; Bracher, Franz; Letters in Organic Chemistry; vol. 10; 1; (2013); p. 2 – 7;,
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. 29671-92-9, name is Carbamimidic chloride hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of Carbamimidic chloride hydrochloride

Step 3; 2-Amino-6- (2,4-difluorophenoxymethyl)benzonitrile mg; 0.46 mmol) and chloroformamidine hydrochloride (80.0 mg, 0.70 mmol) were heated at 140 C in diglyme for 3 hours. The reaction mixture was diluted with water, stirred for 2 hours, filtered, washed with water and dried. Purification by silica gel chromatography (5% methanol in dichloromethane) yielded 72 mg of 5-(2,4- difluorophenoxymethyl) quinazoline-2,4-diamine.

The synthetic route of 29671-92-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DECODE CHEMISTRY, INC.; SINGH, Jasbir; GURNEY, Mark E.; WO2005/123724; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 2533-69-9, A common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, molecular formula is C3H4Cl3NO, 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.

Methyl 3,4-diaminobenzoate (3.3 g, 19.9 mmol) was dissolved in anhydrous MeOH (100 mL). O-Methyl-1,1,1-trichloroacetimidat (1.75 g, 1.25 mL, 9.9 mmol) was added to the resultant solution. Reaction mixture was stirred for 48 h at ambient conditions. A precipitate formed was filtered off, washed with methanol (2×20 mL) and dried in vacuum to a constant weight. Yield 1.0 g (28%).

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; CRYSOPTIX KK; US2010/279122; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics