HRID1613225

反应详情

EQUATION

反应方程式

HRID 1613225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9,10-Dihydro-9,10-ethanoanthracene-11-methanol (1.2 gm), imidazole (0.7 gm) and chlorodiphenylphosphine (1.4 gm) were combined in toluene (80 ml) and treated dropwise with bromine (1.0 gm). The mixture was stirred 10 minutes, then extracted with 10% sodium hydroxide (50 ml) and water (50 ml). The toluene was removed on a rotary evaporator and the residue was dissolved in 1:1 methylene chloride/hexane and placed on a silica gel column. The column was eluted with 1:1 methylene chloride/hexane and the eluant removed on a rotary evaporator to give the product.

WORKUP

后处理

  1. extractionextracted with 10% sodium hydroxide (50 ml) and water (50 ml)
  2. customThe toluene was removed on a rotary evaporator
  3. dissolutionthe residue was dissolved in 1:1 methylene chloride/hexane
  4. washThe column was eluted with 1:1 methylene chloride/hexane
  5. customthe eluant removed on a rotary evaporator
  6. customto give the product