HRID1295952

反应详情

EQUATION

反应方程式

HRID 1295952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1-[3-(tert-Butyl)-4-hydroxyphenyl]-1-ethanone (739 g) was added to a mixture of 69% nitric acid (354 g), water (1 l) and methylene chloride (2 l) at 10° C. to 15° C. while stirring. After then adding diethyl ether (3 l) and acetic anhydride (28 ml), 5 N hydrochloric acid was further added at 10° C. to 15° C. The temperature of the reaction mixture was raised to room temperature over a period of 1.5 hours, and the mixture was then poured into ice water. The mixture was extracted with diethyl ether, and the organic layer was washed with brine and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to yield the title compound (894 g) as a yellow oil.

WORKUP

后处理

  1. extractionThe mixture was extracted with diethyl ether
  2. washthe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure