HRID618224

反应详情

EQUATION

反应方程式

HRID 618224 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7.5 g of (4-hydroxy-phenoxy)-acetonitrile dissolved in 60 ml of nitromethane was cooled in an ice bath and 3.88 ml of 70% nitric acid was added dropwise. After 45 minutes, the reaction mixture was poured into ethyl acetate, washed with brine, dried (MgSO4), and evaporated to dryness. The crude product was purified by silica gel chromatography eluting with ethyl acetate/hexane (1:3), giving 5.45 g of (4-hydroxy-3-nitro-phenoxy)-acetonitrile as a yellow solid, mp 113.1-114.1° C.

WORKUP

后处理

  1. temperaturewas cooled in an ice bath
  2. washwashed with brine
  3. dry with materialdried (MgSO4)
  4. customevaporated to dryness
  5. customThe crude product was purified by silica gel chromatography
  6. washeluting with ethyl acetate/hexane (1:3)