HRID1662953

反应详情

EQUATION

反应方程式

HRID 1662953 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

18 mL fuming nitric acid are added dropwise to a solution of 81.5 g (0.34 mol) 1-(5-benzyloxy-2-hydroxyphenyl)-ethanone in 700 mL acetic acid while cooling with the ice bath, so that the temperature does not exceed 20° C. Then the reaction mixture is stirred for two hours at ambient temperature, poured onto ice water and filtered. The product is recrystallized from isopropanol, suction filtered and washed with isopropanol and diisopropylether. Yield: 69.6 g (72%); mass spectroscopy [M+H]+=288.

WORKUP

后处理

  1. customdoes not exceed 20° C
  2. additionpoured onto ice water
  3. filtrationfiltered
  4. customThe product is recrystallized from isopropanol, suction
  5. filtrationfiltered
  6. washwashed with isopropanol and diisopropylether