HRID652057

反应详情

EQUATION

反应方程式

HRID 652057 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

1-(4-Pyridyl)-1-bromo-2-butanone (28.8 g, 0.1 mol) and 1-acetyl-2-thiourea (13.0 g, 0.11 mol) are combined in 200 ml absolute ethanol and refluxed 24 hours. The solvent is evaporated and the residue is purified by chromatography. The thiol is mixed with (8.1 g, 0.1 mol) potassium cyanate and 0.2 mol 10% aqueous hydrochloric acid. The mixture is heated to 80° C. for 15 minutes, then cooled. The acid is adjusted to ph=6.5 with solid sodium bicarbonate which causes the product to precipitate.

WORKUP

后处理

  1. temperaturerefluxed 24 hours
  2. customThe solvent is evaporated
  3. customthe residue is purified by chromatography
  4. temperaturecooled
  5. customto precipitate