Month: August 2021

Electric Literature of 26487-67-2, 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. 26487-67-2, name is 1-(2-Chloroethyl)azepane hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 1,1-bis(4-hydroxyphenyl)-2-methylprop-1-ene (19.2 mg, 79.9 mumol) in DMF (0.80 mL) at 0 °C was added 60percent sodium hydride (dispersion in paraffin liquid, 25.6 mg, 0.640 mmol). The reaction mixture was stirred for 15 min at 50 °C and then N-(2-chloroethyl)hexahydro-1H-azepine hydrochloride (52.3 mg, 0.264 mmol) was added in portions at room temperature. After the reaction mixture had been stirred for 3 h at 50 °C, saturated aqueous ammonium chloride was added at 0 °C. The mixture was extracted with dichloromethane and the organic layer was dried over sodium sulfate. After filtration of the mixture and evaporation of the solvent, the crude product was purified by thin layer chromatography on silica (eluant; ammoniacal chloroform/methanol = 15/1) to afford RID-F-S*9 (compound 21) (32.9 mg, 84percent) as a pale yellow oil

The chemical industry reduces the impact on the environment during synthesis 1-(2-Chloroethyl)azepane hydrochloride. I believe this compound will play a more active role in future production and life.

Reference:
Article; Hasegawa, Makoto; Yasuda, Yukari; Tanaka, Makoto; Nakata, Kenya; Umeda, Eri; Wang, Yanwen; Watanabe, Chihiro; Uetake, Shoko; Kunoh, Tatsuki; Shionyu, Masafumi; Sasaki, Ryuzo; Shiina, Isamu; Mizukami, Tamio; European Journal of Medicinal Chemistry; vol. 71; (2014); p. 290 – 305;,
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. 6940-78-9, name is 1-Bromo-4-chlorobutane, This compound has unique chemical properties. The synthetic route is as follows., name: 1-Bromo-4-chlorobutane

A mixture of 1-1 [2-(trifluoromethyl)-l0i7-phenothiazine] (300 mg, 1.12 mmol), 1- bromo-4-chlorobutane (391 mg, 2.28 mmol) and CS2CO3 (1.04 g, 3.19 mmol) in DMF (15 mL) was stirred at rt overnight. The mixture was poured into cool water (20 mL) and extracted with EtOAc (15 mL x 3). The combined organic extracts were washed with brine, dried over NaiSCE. fdtered and concentrated under reduced pressure. The residue was purified by column chromatography (petrol ether: EtOAc =10: 1) to provide a yellow solid (240 mg, 60% yield). LC-MS: Rt = 2.30 min; ESI, m/r 358 [M + 1] +

According to the analysis of related databases, 6940-78-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; CAMP4 THERAPEUTICS CORPORATION; BUMCROT, David, A.; SEHGAL, Alfica; HERTZOG, Donald L.; (172 pag.)WO2019/195789; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 51419-59-1, These common heterocyclic compound, 51419-59-1, name is p-Tolylmethanesulfonyl chloride, 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: 5-Chloro-2-nitroaniline (173 mg, 1 mmol) was dissolved in DMF (3 mL) and dry sodium hydride (120 mg, 5 mmol) was added.The obtained mixture was stirred for 1 min and the suitable substitutedbenzenesulfonyl chloride 1 (a?g) or phenylethanesulfonylchloride 3 (a?g) (1,5 mmol) was added in several portions. The reaction was quenched after 2?6 h through the addition of a saturated NaHCO3 aqueous solution (5 mL). The mixture was extractedwith EtOAc (3 10 mL) and dried over Na2SO4. After removal ofthe solvent under reduced pressure, the residue was purified byflash chromatography using cyclohexane/AcOEt (80:20) as eluentand crystallized from Et2O.

The synthetic route of 51419-59-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ferro, Stefania; Buemi, Maria Rosa; De Luca, Laura; Agharbaoui, Fatima E.; Pannecouque, Christophe; Monforte, Anna-Maria; Bioorganic and Medicinal Chemistry; vol. 25; 14; (2017); p. 3861 – 3870;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

69695-61-0, name is 2-Chloro-4-(trifluoromethoxy)aniline, 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. Recommanded Product: 2-Chloro-4-(trifluoromethoxy)aniline

a) 2-Chloro-4-trifluoromethoxybenzenesulfonyl chloride 2-Chloro-4-trifluoromethoxyaniline is reacted to give the corresponding sulfonyl chloride by the same protocol as in Example 6a).

The synthetic route of 69695-61-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI-AVENTIS DEUTSCHLAND GMBH; US2007/197539; (2007); 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

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

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

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;,
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. 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

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;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics