Author: Jessica.F

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. 34813-49-5, name is 2-Methylpropane-2-sulfonamide, A new synthetic method of this compound is introduced below., Recommanded Product: 34813-49-5

Example 11.1N-{4-[(3,5-Dimethyl-4-{[(2-methylpropane-2-sulfonyl)carbamoyl]methyl}-1H-pyrazol-1-yl)methyl]phenyl}-4-(trifluoromethyl)benzamide{3,5-Dimethyl-1-[4-(4-trifluoromethyl-benzoylamino)-benzyl]-1H-pyrazol-4-yl}-acetic acid (example 1.1, 250 mg, 0.58 mmol), 2-methylpropane-2-sulfonamide (95 mg, 0.70 mmol), 1,3-dicyclohexylcarbodiimid (143 mg, 0.70 mmol) and 4-dimethylaminopyridine (85 mg, 0.70 mmol) in 2.5 ml dichloromethane were stirred for 3 h at 30 C. The solvent was removed under reduced pressure and the residue was purified by MPLC (silica gel, CH2Cl2/methanol 95:5).Yield: 51 mgESI mass spectrum: [M+H]+=551Retention time HPLC: 1.34 min (method D).

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; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2012/28938; (2012); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 85175-59-3, name is 3-(3-Chloropropyl)-1,3-dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one, molecular formula is C15H18ClNO3, 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. Formula: C15H18ClNO3

EXAMPLE 1 1-[7,8-Dimethoxy-1,3-dihydro-2H-3-benzazepin-2-on-3-yl]-3-[N-methyl-N-(6,7-dimethoxy-1,2,3,4,-tetrahydronaphth-2-yl)-amino]-propane A mixture of 2-methylamino-6,7-dimethoxy-1,2,3,4-tetrahydronaphthalene (1.72 g, 0.0078 mol), triethylamine (1.09 ml, 0.0078 mol) and 1-(7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-on-3-yl)-3-chloropropane (2.3 g, 0.0078 mol) is heated to a reaction temperature of 90 C. in steps within one hour and kept at this temperature for 2 hours. The initial suspension slowly changes into a clear solution and begins to precipitate in a jelly-like manner after about 30 minutes. The cooled reaction mixture is dissolved in 0.5M sodium hydroxide solution/ethyl acetate, the organic phase is washed with water, dried over magnesium sulphate, concentrated by evaporation in vacuo and purified over alumina (300 g), neutral, activity II, with methylene chloride and then with increasing quantities of ethanol (up to 20%). The hydrochloride is precipitated from a solution in acetone using ethereal hydrochloric acid. Yield: 1.39 g Mp: >125 C. (Decomp.).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 85175-59-3, its application will become more common.

Reference:
Patent; Dr. Karl Thomae GmbH; US4584293; (1986); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 782-45-6, 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 782-45-6 as follows.

Stage 1: 4-[(2-chloro-9H-purin-6-yl]amino]-N-phenylbenzamide The procedure is carried out as in Example 1, starting with 195 mg of 2,6-dichloropurine, 5 ml of butanol and 272 mg of 4-amino-N-phenylbenzamide. 360 mg of the expected product are thus obtained.

According to the analysis of related databases, 782-45-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Aventis Pharma S.A.; US2004/63732; (2004); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 209917-48-6, name is N-tert-Butyl 4-Aminophenylsulfonamide, belongs to amides-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 209917-48-6, Product Details of 209917-48-6

A mixture of substituted 2,4-dichloropyrimidine (1.0 equiv.) and substituted aniline (1.15 equiv.) in MeOH/water (1 : 1.5, 0.2 M) was stirred at 45 C. The reaction time is indicated below. Upon cooling to ambient temperature, the desired product precipitated and was filtered, washed with MeOH/water (1 : 1.5, 20 mL), and dried. 2,5-Dichloro-/Y4-(4-[/Y-(l,l-dimethylethyl)sulfamoyl]phenyl)pyrimidin-4-amine (SG1-182): This was prepared from 2,4,5-trichloropyrimidine (0.500 g) and SG1-177 (0.715 g) using procedure A (stirred for 4 d). The crude solid was purified via flash chromatography (S1O2) eluting with hexanes/EtOAc (0: 10 to 4:6 v/v) to provide the title compound as a tangerine-colored solid (0.590 g, 58%). Mp: 180-181 C. NMR (400 MHz, DMSO-ifc): delta 9.73 (s, IH, disappeared on D20 shake), 8.46 (s, IH), 7.80 (s, 4H), 7.48 (s, IH, disappeared on D20 shake), 1.09 (s, 9H). HPLC-MS (ESI+): m/z 773.1 [10%, (MCl35Cl37+M35Cl35Cl+Na)+], 379.1 [10%, (MC137C137+H)+], 377.1 [70%, (MC135C137+H)+], 375.1 [100%, (M35C135C1+H)+].

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, N-tert-Butyl 4-Aminophenylsulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; H. LEE MOFFITT CANCER CENTER & RESEARCH INSTITUTE, INC.; SCHOeNBRUNN, Ernst; LAWRENCE, Nicholas J.; LAWRENCE, Harshani R.; (293 pag.)WO2017/66428; (2017); A1;,
Amide – Wikipedia,
Amide – 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. 37073-15-7, name is 1-(Methylsulfonyl)-1H-benzo[d][1,2,3]triazole belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C7H7N3O2S

General procedure: A mixture of alpha,beta-unsaturated aromatic or aliphatic acid (10 mmol), CH3SO2Bt (10 mmol) and Et3N (15 mmol) were refluxed in dry THF (50 mL) overnight. The solvent was evaporated and the residue was dissolved in CH2Cl2 (100 mL). The organic phase was washed with brine (3 times) and dried over anhydrous Na2SO4. The organic phase was concentrated under vacuum to give a crude product, which could be further purified by recrystallization from a proper solvent.

The synthetic route of 37073-15-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Xia, Ziming; Lv, Xin; Wang, Wencun; Wang, Xiaoxia; Tetrahedron Letters; vol. 52; 38; (2011); p. 4906 – 4910;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 94838-59-2, 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. 94838-59-2 name is tert-Butyl 4-aminophenethylcarbamate, 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.

A solution of formaldehyde (0.303 g, 4 mmol, 40% in water), fert-butyl 4- aminophenethylcarbamate (1.135 g, 4.8 mmol) and NaBH3CN (1.257 g, 20 mmol) in methanol (14 mL) was stirred at room temperature for 4 h. Water (30 mL) was added to the reaction mixture afterward and the mixture was extracted with ethyl acetate (30 mL 3). The organic layer was washed with water (20 mL) and brine (20 mL), dried with NaiSCri and concentrated. The residue was purified by column chromatography to afford the title compound as colorless oil (0.337 g, 33.7 % yield). NMR (500 MHz, DMSO-riri) d: (d, J= 8.3 Hz, 2H), 6.79 (t, J= 5.3 Hz, 1H), 6.46 (d, J= 8.4 Hz, 2H), 5.41 (q, J= 5.0 Hz, 1H), 3.03 (dd, J= 14.9, 6.1 Hz, 2H), 2.64 (d, J= 5.2 Hz, 3H), 2.54 – 2.51 (m, 2H), 1.38 (s, 9H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl 4-aminophenethylcarbamate, and friends who are interested can also refer to it.

Reference:
Patent; ZHEJIANG VIMGREEN PHARMACEUTICALS, LTD; SUN, Sanxing; ZHAO, Long; HU, Chongbo; CHEN, Zhengshu; YE, Jinqi; (0 pag.)WO2020/2969; (2020); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 120157-97-3, 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. 120157-97-3, name is N-Boc-2-(4-Bromophenyl)ethylamine belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[2- (4-Bromo-phenyl)-ethyl]-carbamic acid tert-butyl ester (1. 5g, 4.99 mmol) was dissolved in toluene (0.2 M) in a 100 mL round-bottom flask. To this was added LiCl (10.6 mg, 0.25 mmol, 0. 05eq) and the resulting solution was flushed under nitrogen for 2-3 minutes. PdCl2 (PPh3) 2 (175.4 mg, 0. 25mmol, 0. 05eq) was added to the reaction mixture and the solution was again flushed under nitrogen for 2-3 minutes. 2-Tributylstannanyl-pyridine, from Frontier (1. 84g, 4.99mmol, leq) was added last and the reaction mixture was heated to 110C overnight. The solvent was removed under vacuum. The crude material was purified on column chromatography (silica gel), and eluted with EtOAc-Hexanes 15: 85 to afford [2- (4-Pyridin-2-yl-phenyl)-ethyl]-carbamic acid tert-butyl ester in good yield.

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, N-Boc-2-(4-Bromophenyl)ethylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; WO2003/93245; (2003); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Some common heterocyclic compound, 112101-81-2, name is R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide, molecular formula is C10H16N2O3S, 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. name: R-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide

EXAMPLE 34 R-(-)-5-[2-[2-(5-Fluoro-2-methoxyphenoxy)-ethylamino]propyl]-2-methoxybenzenesulfonamide hydrochloride A suspension of 1.00 g of R-(-)-5-(2-aminopropyl)-2-methoxybenzenesulfonamide [[alpha]D25 -13.8 (C=1,MeOH), m.p.156.5-160.5 C. (H2 O) ] 11.00 g of 2-(2-bromoethoxy)-4-fluoroanisole and 0.20 g of potassium iodide in 40 ml of N,N-dimethylformamide was heated for 10 hours at 85 C. After cooling, the reaction mixture was poured into water, made alkaline with 10% sodium hydroxide aqueous solution and extracted with ethyl acetate. The extract was washed with water, dried and evaporated. The residue was chromatographed on silica gel using chloroform-methanol (9:1) as an eluant to give 0.81 g of the free base as colorless crystals which were recrystallized from methanol as colorless needles, m.p.144-145 C. Analysis for C19 H25 FN2 O5 S: Calculated %: C, 55.33; H, 6.11; N, 6.79. Found %: C, 55.20; H, 5.93; N, 6.54.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 112101-81-2, its application will become more common.

Reference:
Patent; Hokuriku Pharmaceutical Co., Ltd.; US4971990; (1990); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 121492-06-6, 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 121492-06-6 as follows.

General procedure: To a solution of acid 7(a-p) (1 equiv) and amine (1.5 equiv) in dichloromethane were added HoBt (1.5 equiv) and EDCI(1.5 equiv). The reaction mixture was stirred at room temperature overnight, then washed with 5% aqueous HCl, 5% aqueous sodium bicarbonate, water, and brine, and dried. Purification by chromatography afforded 8-9(a-c).

According to the analysis of related databases, 121492-06-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Yang, Ying-Rui; Wei, Jin-Lian; Mo, Xiao-Fei; Yuan, Zhen-Wei; Wang, Jia-Lin; Zhang, Chao; Xie, Yi-Yue; You, Qi-Dong; Sun, Hao-Peng; Bioorganic and Medicinal Chemistry Letters; vol. 26; 11; (2016); p. 2713 – 2718;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 103361-99-5, These common heterocyclic compound, 103361-99-5, name is 7-Fluoro-2H-benzo[b][1,4]oxazin-3(4H)-one, 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.

Step A 6-Iodo-7-fluoro-2H-1,4-benzoxazin-3(4H)-one 7-Fluoro-2H-1,4-benzoxazin-3(4H)-one (15.8 g) was mixed with iodine monochloride (15.6 g) in acetic acid (150 ml) and heated to reflux for 36 h. The cooled mixture was treated with saturated aqueous sodium bisulfite until the color was dissipated. The solid was filtered and washed well with water. The solid was air dried and dried further by dissolution in dimethylformamide (100 ml) and evaporated to dryness under reduced pressure to give the desired product (26.3 g) contaminated with some starting material. (The reaction can be taken to completion by addition of more iodine monochloride and refluxing for 24 h longer.) The crude product was used in Step B.

The synthetic route of 103361-99-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. I. Du Pont de Nemours and Company; US5670455; (1997); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics