HRID900733

反应详情

EQUATION

反应方程式

HRID 900733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ammonium dithiocarbamate (0.444 g, 4.03 mmol) was added to 2-bromo-1-(4-pyridinyl)-1-ethanone hydrobromide (1.03 g, 3.67 mmol) in ethanol (10 ml and stirring continued at room temperature for 18 hr. The solid was filtered and re-crystallized from methanol to give 4-pyridin-4-yl-thiazole-2-thiol. This thiol (272 mg, 1.39 mmol) was then coupled with N1-3-chlorophenyl)-2-chloroacetamide (284 mg, 1.39 mmol) as described in earlier examples, in acetonitrile in the presence of triethylamine (0.580 ml, 4.2 mmol) to afford crude product. This was purified by reverse phase HPLC to afford N-(3-Chloro-phenyl)-2-(4-pyridin-4-yl-thiazol-2-ylsulfanyl)-acetamide. MS (ES) 363 (M+H)+

WORKUP

后处理

  1. filtrationThe solid was filtered
  2. customre-crystallized from methanol