HRID1197431

反应详情

EQUATION

反应方程式

HRID 1197431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of potassium tert-butoxide (8.56 g, 0.076 mol) in ethanol (75 mL) was added 2(R,S)-aminopropanethiol (3.1 g, 0.0246 mol) and ethyl 2-chloro-5-sulfamoylthiophene-3-carboxylate (5.98 g, 0.022 mol). The mixture was heated at reflux for 24 hours, and then allowed to stand at room temperature for 24 hours. Following removal of most of the solvent by vacuum concentration, the mixture was acidified to pH 3 with dilute hydrochloric acid. The resulting solids were removed by filtration and dried to give 4.44 g of the title compound, mp 184°-187° C.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 24 hours
  3. customremoval of most of the solvent
  4. concentrationby vacuum concentration
  5. customThe resulting solids were removed by filtration
  6. customdried