一二三四区视频,亚洲少妇熟女色,日本久热无码视频网,欧美国产日韩大尺度,亚洲a视频,久久少妇一区二区,日韩999无码视频,刺激久久久久久久,啊啊啊啊不要啊在线

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List Isonicotinamide
1453-82-3

Isonicotinamide synthesis

13synthesis methods
synthesis of isonicotinamide: In 6g tert-amyl alcohol, add 100mg ferric oxide, 100mg cobalt tetroxide and 100mg manganese dioxide (mass percentage in the mixture: 4.6%), 60mg 4-cyanopyridine (mass percentage in the mixture: 0.91%), 200uL Water (mass percentage in the mixture: 3.0%), mix well; react at 80°C for 24 hours, the conversion rate of 4-cyanopyridine is 99.0%, and the selectivity of the corresponding Isonicotinamide is 99.0%.
-

Yield:1453-82-3 95%

Reaction Conditions:

Stage #1: pyridine-4-carboxylic acidwith chloroformic acid ethyl ester;triethylamine in tetrahydrofuran at 0; for 0.5 h;
Stage #2: with ammonium chloride in tetrahydrofuran;water at 0; for 0.5 h;

Steps:

4.2.11 4.2. Typical procedure for the primary amidation of 3-phenylpropanoic acid 1a with NH4Cl

General procedure: To a colorless solution of 75mg (0.50mmol) of 3-phenylpropanoic acid 1a in 10mL of THF were added at 0°C 67μL (0.70mmol, 1.4equiv) of ClCO2Et and 209μL (1.5mmol, 3.0equiv) of Et3N.
After stirring for 30min at 0°C, 0.75 ml of a 1.0M aqueous solution of NH4Cl (0.75mmol, 1.5equiv) was added at 0°C to the colorless suspension.
The mixture was stirred for 30min at 0°C and 5mL of H2O was added to the resulted mixture.
The colorless clear solution was extracted with 30mL of EtOAc and the aqueous layer was extracted with 20mL of EtOAc.
The organic layers were combined, washed with 5mL of brine, and dried over anhydrous MgSO4.
The crude product was chromatographed on silica gel with EtOAc to afford 72mg (96% yield) of 3-phenylpropanamide 2a. 4.2.11
Isonicotinamide 2k
58?mg (95%); colorless solid; mp: 151-153?°C; 1H NMR (400?MHz, DMSO-d6): δ 7.73 (br, 1H, NHA), 7.76, 8.72 (d, d, J?=?6.0, 6.0?Hz, 2H, 2H, pyridyl), 8.25 (br, 1H, NHB); 13C NMR (100?MHz, DMSO-d6): δ 121.3, 141.2, 150.1, 166.2; IR (KBr, vmax/cm-1)?=?3334 (CONH), 1684 (CON), 1624 (CON); HRMS (ESI-TOF): Calcd for C6H7N2O (M+H)+: 123.0553, found: 123.0529.

References:

Ezawa, Tetsuya;Kawashima, Yuya;Noguchi, Takuya;Jung, Seunghee;Imai, Nobuyuki [Tetrahedron Asymmetry,2017,vol. 28,# 12,p. 1690 - 1699]

Isonicotinamide Related Search:

永泰县| 营口市| 麻城市| 定兴县| 桃源县| 营口市| 丰宁| 五常市| 英超| 元江| 洞口县| 靖安县| 康保县| 龙口市| 中阳县| 革吉县| 辰溪县| 南涧| 利津县| 湟中县| 抚顺市| 新邵县| 嘉黎县| 浮山县| 通化县| 辉县市| 滕州市| 兴业县| 团风县| 黄骅市| 津南区| 武邑县| 龙井市| 桐庐县| 大港区| 莎车县| 墨玉县| 陆川县| 龙口市| 台中市| 靖边县|