HRID2408951

反应详情

EQUATION

反应方程式

HRID 2408951 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 (appr. 25 mL) 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 a off-white color solid (1.8 g, 83%), mp 160-162° C. 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

  1. temperaturethe mixture refluxed for 1 h
  2. distillationEthanol was distilled off under vacuum (appr. 25 mL)
  3. filtrationThe separated crystals were filtered off
  4. washwashed with cold water
  5. customdried