Month: January 2021

Synthetic Route of 162576-01-4, 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. 162576-01-4, name is Benzyl (2-aminoethyl)(methyl)carbamate hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

Boc-Arg (Pbf) -OH (16.0 g, ca. 30.4 mmol) in DMF (150 mL)Compound CA solution of hydrochloride (8.2 g, 33.4 mmol) and DIEA (16.9 mL, 97.2 mmol) was cooled in an ice bath followed by a solution of HATU (13.8 g, 36.4 mmol) dropwise In 20 minutes. The temperature of the reaction mixture was raised to ambient temperature and stirring was continued for an additional hour. The reaction mixture was diluted with EtOAc (1 L) and extracted with water (3 ¡Á 200 mL) and brine (200 mL). The organic layer was dried over MgSO 4 and evaporated to give compound D (24.4 g, yield exceeding the quantitative value) as a yellowish oil.

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

Reference:
Patent; SIGNATURE THERAPEUTICS INCORPORATED; JENKINS, THOMAS E; Husfeld, Craig O; Seroogy, Julie D; Wray, Jonathan W; (162 pag.)JP2016/41698; (2016); A;,
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. 5202-85-7, name is 2-Amino-5-chlorobenzamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C7H7ClN2O

General procedure: To an oven-dried 20 cm3 test tube with a ground-in stopperequipped with a stir bar were added anthranilamide (1.0 mmol), benzyl alcohol (1.0 mmol), KOH (2.0 mmol),and 4 cm3 toluene. The test tube was put in an oil bath potpreheated at 90 C and the mixture was stirred for 20 h at90 C. After cooling to room temperature, the reactionmixture was added about 5 g silica gel and directly condensedon a rotator under vacuum. The resulting residualwas transferred to a silica gel chromatography column andeluted with a solution of petroleum ether and ethyl acetate[4/1 (v/v)] to give a white solid 2-phenyl-4(3H)-quinazolinone.For some products (3f, 3g, 3n, and 3t) onlysparingly soluble in ethyl acetate, the reaction mixtureswere condensed in vacuo on a rotary evaporator. Theresiduals were washed three times with water and oncewith ethyl acetate, and then dried in an infrared oven togive the desired products pure enough for NMR analysis.

The synthetic route of 5202-85-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Qiu, Dezhi; Wang, Yanyan; Lu, Dongming; Zhou, Lihong; Zeng, Qingle; Monatshefte fur Chemie; vol. 146; 8; (2015); p. 1343 – 1347;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 40724-47-8, 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 40724-47-8 as follows.

[0216] In a microwave tube was placed ethyl 2-(5-fluoro-3-(4,4,5,5-tetramethyl-1,3,2- dioxaborolan-2-yl)- 1H-indol- 1 -yl)thiazole-4-carboxylate (114 mg, 0.15 mmol, ?55percent purity), 4-(bromomethyl)benzenesulfonamide (49.9 mg, 0.200 mmol), and Pd(Ph3P)4 (17.33 mg,0.0 15 mmol). The tube was sealed and air was removed and re-filled with N2 (2-3 times). A mixture of toluene (0.75 ml, ratio: 2.500)/EtOH (0.3 ml, ratio: 1.000) was added, and then 2 N Na2CO3(aq) (0.3 mL, 0.6 mmol, 4 equiv) was added. The mixture was stirred at 80 ¡ãC (preheated) for 2 h. The organic layer was separated, and the aqueous layer was extracted with EtOAc (2 mL x 3). The combined organic layer was dried (Na2504) and filtered. After removal of the solvent, the product was purified by silica gel chromatography using 20-50percent EtOAc/hexane as the eluent to give ethyl 2-(5-fluoro-3-(4-sulfamoylbenzyl)-1H-indol-1- yl)thiazole-4-carboxylate (47 mg, 0.102 mmol, 68.2percent yield) as a white solid.

According to the analysis of related databases, 40724-47-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THE UNITED STATES OF AMERICA AS REPRESENTED BY THE SECRETARY, DEPARTMENT OF HEALTH AND HUMAN SERVICES; VANDERBILT UNIVERSITY; MALONEY, David J.; JADHAV, Ajit; BANTUKALLU, Ganesha Rai; BRIMACOMBE, Kyle Ryan; MOTT, Bryan T.; YANG, Shyh Ming; URBAN, Daniel Jason; HU, Xin; SIMEONOV, Anton; KOUZNETSOVA, Jennifer L.; WATERSON, Alex Gregory; SULIKOWSKI, Gary Allen; KIM, Kwangho; CHRISTOV, Plamen; JANA, Somnath; (387 pag.)WO2016/109559; (2016); A2;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 749927-69-3, The chemical industry reduces the impact on the environment during synthesis 749927-69-3, name is 4-Bromo-2-fluoro-N-methylbenzamide, I believe this compound will play a more active role in future production and life.

N-methyl-2-fluoro-4-bromo-benzamide 1a (23.21 g, 100 mmol) was added to a three-necked flask.Cyclobutyrate hydrochloride 2 (15.16 100 mmol) and N,N-dimethylacetamide (116 mL),Copper iodide (1.90 g, 10 mmol) and cesium carbonate (71.68 g, 220 mmol) were added under a nitrogen atmosphere, and the mixture was stirred and heated to 90 to 95 C overnight.At the end of the reaction, water (232 mL) and isopropyl acetate (232 mL) were added, and the mixture was stirred and the aqueous phase was collected, and the pH was adjusted to 3 to 4 with 4N hydrochloric acid.Precipitating a large amount of solids,Filtration dried to give compound 3 (17.88 g, 79%).

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-Bromo-2-fluoro-N-methylbenzamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hangzhou Kechao Biological Technology Co., Ltd.; Zheng Xuchun; Zhang Yiping; (10 pag.)CN108383749; (2018); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 72505-21-6, These common heterocyclic compound, 72505-21-6, name is 4-(Trifluoromethyl)thiobenzamide, 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.

Intermediate Example P; EMI70.1Ethyl 4- (1-methylethyl)-2- [4- (trifluoromethyl) phenyl]-1, 3-thiazole-5-carboxylate(XI-5a) Ethyl isobutyrylacetate(XI-3a) (3.006 g, 19.0mmol) was dissolved in chloroform (20 mL). Sulfuryl chloride (1.70 mL, 21.2mmol) was added and the solution was stirred at RT for 18 hours, then was concentrated. The residue was dissolved in ethanol (50 mL).4- (Trifluoromethyl) benzenethioamide (4.234 g, 20.6mmol) was added and the solution was heated to reflux for 24 hours. The mixture was cooled to RT and filtered. The solid was washed with cold ethanol and dried to provide the title product (2.68 g, 32%) as a pale yellowsolid.’H NMR (400 MHz,CDCI3)6 8.09 (d, J= 8.1 Hz, 2H), 7.69 (d, J= 8.1 Hz, 2H), 4.35 (q, J= 7.1 Hz, 2H), 3.99 (qu, J= 6.8 Hz,1H), 1.39 (t, J= 7.1 Hz,3H), 1.35 (d, J= 6.8 Hz, 6H).

Statistics shows that 4-(Trifluoromethyl)thiobenzamide is playing an increasingly important role. we look forward to future research findings about 72505-21-6.

Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2005/51890; (2005); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 6292-59-7, 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. 6292-59-7, name is 4-(tert-Butyl)benzenesulfonamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a stirred solution of glucal (1 equiv.) and N-nucleophile (1.1 equiv.) inanhydrous 1,2-dichloroethanne (2 mL/mmol) under an atmosphere of argon was added Zn(OTf)2 (10 molpercent) at 40?C. The reaction mixture was stirred untilthe complete consumption of the starting material (glycal). The solvent wasfiltered and concentrated in vacuo, and the crude residue was redissolved indichloromethane and loaded on a silica gel column. The product was purified by silica gel column chromatography using hexane/EtOAc as the eluent to affordthe 2,3-unsaturated N-glycosides. All of the products were confirmed by1H NMR, 13C NMR, and MS/HRMS spectroscopy and compared with that of literature data; characterization data of new products are outlined in the experimentalsection

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-(tert-Butyl)benzenesulfonamide, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Reddy, Thurpu Raghavender; Battina, Suresh Kumar; Kashyap, Sudhir; Journal of Carbohydrate Chemistry; vol. 34; 3; (2015); p. 133 – 144;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Related Products of 53844-02-3, 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. 53844-02-3, name is Benzyl (2-bromoethyl)carbamate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of 1 (15.0mmol) in CH3CN (60mL) were added K2CO3 (3.10g, 22.5mmol) and N-Cbz-2-bromoethylamine (3.87g, 15.0mmol) under stirring. It was then kept at 80C, and monitored by TLC (Hexane/EtOAc=2/1, v/v). Next, K2CO3 was removed by filtration. The filtrate was concentrated to give a light brown oil. The oil was dissolved in ethyl acetate (150mL) and the solution was washed with water (2¡Á50mL). The organic phase was dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford the crude product. The residue was concentrated and purified by silica gel column chromatography (Hexane/EtOAc=4/1, v/v) to give a white solid

The synthetic route of Benzyl (2-bromoethyl)carbamate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Ao, Chunyan; Men, Jian; Wang, Yang; Shao, Tao; Huang, Yuanyuan; Huo, Junji; Gao, Guowei; Tetrahedron Asymmetry; vol. 27; 13; (2016); p. 589 – 595;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 138-41-0, name is Carzenide, 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. Safety of Carzenide

Compound 3-7 (300 mg, 1.33 mmol), p-sulfonamide benzoic acid (294 mg, 1.46 mmol, 1.1 eq.), HOBt (539 mg, 3.99 mmol, 3 eq.) and EDCI (765 mg, 3.99 mmol, 3 eq.) in 50 mL Single mouth bottle,DMF and TEA (0.74 mL, 5.32 mmol, 4 eq.) were added.Stir at room temperature overnight. TLC tracking monitoring. Rotate the DMF,Add EA and water for extraction, wash with saturated brine, dry, spin dry, and pass through column (DCM:acetone = 3:1). A white solid of 450 mg was obtained in a yield of 83%.

The synthetic route of Carzenide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Guangzhou Hengnuokang Pharmaceutical Technology Co., Ltd.; Zhang Jiancun; Lin Cai; Zou Qingan; (45 pag.)CN108456208; (2018); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 3984-14-3, These common heterocyclic compound, 3984-14-3, name is N,N-Dimethylsulfamide, 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.

EXAMPLE 5 (+/-)8-cyclohexyl-N-[(dimethylamino)sulfonyl]-1,1a,2,12b-tetrahydro-1a-(4-morpholinylcarbonyl)-cycloprop[d]indolo[2,1-a][2]benzazepine-5-carboxamide. A 2M solution of oxalyl chloride (0.093 mL, 0.186 mmol) in CH2Cl2 was added dropwise to a solution of (+/-)-8-cyclohexyl-1,1a,2,12b-tetrahydro-1a-(4-morpholinylcarbonyl)-cycloprop[d]indolo[2,1-a][2]benzazepine-5-carboxylic acid (45 mg, 0.093 mmol) in CH2Cl2 (10 mL), containing one drop of DMF. The reaction mixture was stirred at rt. for 2 hr., after which it was concentrated and dried under high vacuum. The residue was subsequently dissolved in THF (10 mL) and a solution of N,N-dimethylsulfonamide, (23 mg, 0.186 mmol) and DIPEA (0.049 mL, 0.279 mmol)) in THF (2 mL) was added. This was followed by the addition of DMAP (10 mg), after which the reaction was stirred at rt. for 10 min., and then at 50 C. overnight. It was then cooled, and the mixture concentrated under reduced pressure. The resultant residue was purified by preparative reverse phase HPLC to afford the product as a yellow solid, (5.0 mg, 9% yield). MS m/z 591(MH+), Retention time: 3.525 min; 1H NMR (300 MHz, CD3OD) delta ppm. Compound was observed to exist as inter-converting rotamers, as evidenced from the compound’s NMR spectrum.

The synthetic route of 3984-14-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2007/60565; (2007); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 154350-29-5, These common heterocyclic compound, 154350-29-5, name is Cyclopropanesulfonamide, 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.

To an iced slurry of cyclopropanesulfonamide (1.21 g, 9.99 mmol), Triethylamine (2.95 mL, 20.97 mmol), and 4-Dimethylaminopyridine (0.061 g, 0.499 mmol) in CH2Cl2 (50 mL) was added solution of Di-tert-butyl dicarbonate (2.423 mL, 10.99 mmol) in DCM (10 mL) dropwise. The formed solution was stirred at room temperature overnight, Removed the solvent in vacuo. The residual oil was taken up in EtOAc and washed with 1M HCl and brine. Dried over MgSO4, filtered, and concentrated. The residue was purified by Biotage column, eluted with gradient 5percent50percent acetone-hexane to yield the desired produce tert-butyl cyclopropylsulfonylcarbamate (2.17 g, 9.61 mmol, 96percent yield) as a viscous oil, which solidified upon standing on bench. 1H NMR (400 MHz, CDCl3) ppm 1.11-1.13 (m, 2H) 1.37-1.39 9m, 2H) 1.53 (s, 9H), 2.89-2.92 (m, 1H) 7.00-7.05 (b, NH).

The synthetic route of 154350-29-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2010/150866; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics