HRID386402

反应详情

EQUATION

反应方程式

HRID 386402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-Bromo-furan-2-carboxylic acid hydrazide (20.5 g, 100 mmol) was added to a mixture of potassium hydroxide (6.2 g, 110 mmol) and methanol (125 ml). The mixture was stirred for 30 minutes at room temperature. Carbon disulfide (15.2 g, 200 mmol) was added. The mixture was stirred at reflux for 30 hours. Water (60 ml) was added and the excess of carbon disulfide and methanol was evaporated. The aqueous suspension was acidified by adding concentrated hydrochloric acid (14 ml). The product precipitated and was washed with water (20 ml), dried and evaporated. Yield 8.58 g (35%).

WORKUP

后处理

  1. stirringThe mixture was stirred
  2. temperatureat reflux for 30 hours
  3. customthe excess of carbon disulfide and methanol was evaporated
  4. additionby adding concentrated hydrochloric acid (14 ml)
  5. customThe product precipitated
  6. washwas washed with water (20 ml)
  7. customdried
  8. customevaporated