HRID730179

反应详情

EQUATION

反应方程式

HRID 730179 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 8-bromo-2-methoxy-1-methyl-11,12-dihydro-6H-dibenzo [a,e]cycloocten-5-one 12 (1.0 g: 2.9 mmol), acetic acid and selenium dioxide (0.64 g; 5.8 mmol) was stirred at 150° C. for 2 hr, cooled to room temperature, diluted with dichloromethane and filtered through silica gel to remove the suspended solids. The filtrate was evaporated to dryness. The residue was heated in ethyl acetate and crystallized by adding hexane to give compound 13 as grey needles, 0.71 g, 68% yield.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. filtrationfiltered through silica gel
  3. customto remove the suspended solids
  4. customThe filtrate was evaporated to dryness
  5. temperatureThe residue was heated in ethyl acetate
  6. customcrystallized
  7. additionby adding hexane