HRID1097227
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of 3-amino-4,5,6,7-tetrahydrobenzo[1,2-b]selenophene-2-carbonitrile (2.4 g) in ethanol (50 mL) was added aqueous sodium hydroxide solution (50 mL, 10%) at rt and the mixture was refluxed for 1 h. The cooled reaction mixture was poured into ice cooled water and stirred for 15 min. The precipitated solid filtered, washed with cold water and dried to give the product as a pale brown color solid (1.4 g, 54%), mp 152-154° C. 1H NMR (400 MHz, DMSO-d6): δ 6.58 (1H, s, —CONH2), 6.45 (1H, s, —CONH2), 2.66 (2H, s, H-7), 2.24 (2H, s, H-4), 1.73 (4H, s, H-5,6); LC-MS (positive ion mode): m/z 265, 267 (M+Na)+.
WORKUP
后处理
- temperaturethe mixture was refluxed for 1 h
- customThe cooled reaction mixture
- additionwas poured into ice
- filtrationThe precipitated solid filtered
- washwashed with cold water
- customdried