HRID850964

反应详情

EQUATION

反应方程式

HRID 850964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 60.4 g. of ethyl-5-nitro-2-thiophenecarboxylate and 480 ml. of concentrated hydrochloric acid is cooled in an ice-bath to below -5°. To this mixture is added 72 g. of granular tin in small amounts, keeping the temperature near -5°. After stirring for 6 hours, 575 ml. of 10 N sodium hydroxide is added to neutralize the mixture. Methylene chloride and Celite are added and the mixture is filtered. The methylene chloride layer of the filtrate is separated, dried over sodium sulfate, and filtered through Magnesol. Evaporation affords an oil which is distilled to yield the product.

WORKUP

后处理

  1. additionA mixture of 60.4 g
  2. additionTo this mixture is added 72 g
  3. customnear -5°
  4. filtrationthe mixture is filtered
  5. customThe methylene chloride layer of the filtrate is separated
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered through Magnesol
  8. customEvaporation
  9. customaffords an oil which
  10. distillationis distilled
  11. customto yield the product