HRID264822

反应详情

EQUATION

反应方程式

HRID 264822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 42.0 g of ethyl 2,2-bisfluoromethyl-6-nitro-2H-1-benzopyran-4-carboxylate, 88 g of stannous chloride and 500 ml of ethyl alcohol was heated while refluxing for 2 hours. A 2N aqueous solution of sodium hydroxide was added to the reaction mixture, followed by extracting with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and then concentrated under (reduced pressure to obtain 5,2 g of ethyl 6-amino-2,2-bisfluoromethyl-2H-1-benzopyran-4-carboxylate as an oily substance.

WORKUP

后处理

  1. temperaturewas heated
  2. temperaturewhile refluxing for 2 hours
  3. extractionby extracting with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under (reduced pressure