HRID1529830
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
CONDITIONS
反应条件
- 温度
- 7.5 °C
PROCEDURE
实验过程
To a suspension of 3-amino-5-(tert-butyl)selenophene-2-carbonitrile (2.0 g) in aqueous sodium hydroxide solution (50 mL, 10%) was added ethanol (50 mL) and the mixture refluxed for 1 h. Ethanol was distilled off under vacuum and the mixture was allowed to cool to 5-10° C. The separated crystals were filtered off, washed with cold water and dried to give the product as an off-white color solid (1.8 g, 83%), mp 160-162° C. (Hesse, S.; Chenet, C.; Thomae, D.; Kirsch, G. Synthesis, 2009, 1204-1208). 1H NMR (400 MHz, CDCl3): δ 6.58 (1H, s), 5.75 (2H, br s), 5.13 (2H, br s), 1.34 (9H, s).
WORKUP
后处理
- temperaturethe mixture refluxed for 1 h
- distillationEthanol was distilled off under vacuum
- filtrationThe separated crystals were filtered off
- washwashed with cold water
- customdried
- customto give the product