HRID1977751

反应详情

EQUATION

反应方程式

HRID 1977751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A suspension of 4-(3-nitrophenyl)-2-(3-pyridyl)-thiazole hydrobromide (3.6 g, 10 mmol) in ethanol (150 ml) was treated with a solution of tin (II) chloride (3.7 g, 30 mmol) in concentrated hydrochloric acid (12 ml). The mixture was heated at 50° C. for 16 h. A further portion of tin (II) chloride (2.9 g, 15 mmol) was added and the mixture heated at 50° C. for a further 4 hours before being evaporated to dryness. The residue was partitioned between ethyl acetate and 1M aqueous sodium hydroxide. The ethyl acetate extract was dried (Na2SO4) and filtered through a plug of silica. Evaporation afforded the title compound as a yellow solid (2.15 g, 85%).

WORKUP

后处理

  1. temperaturethe mixture heated at 50° C. for a further 4 hours
  2. custombefore being evaporated to dryness
  3. customThe residue was partitioned between ethyl acetate and 1M aqueous sodium hydroxide
  4. extractionThe ethyl acetate extract
  5. dry with materialwas dried (Na2SO4)
  6. filtrationfiltered through a plug of silica
  7. customEvaporation