HRID485423

反应详情

EQUATION

反应方程式

HRID 485423 的结构方程式

PROCEDURE

实验过程

13.6 G. methyl-11-bromo-10,11-dihydrodibenzo[b,f]thiepin-3-carboxylate is suspended in 150 cc. sulfolane and to the mechanically stirred mixture 7.18 g. sodium borohydride is added in portions over one hour. The foamy mixture is stirred an additional half hour. The mixture is diluted with 1.5 l. of water and extracted with ether. The organic layer is washed with water, dried, evaporated, and the residual oil is chromatographed on silica gel. Elution with benzene affords 8.1 g. of the pure oily material.

WORKUP

后处理

  1. additionThe mixture is diluted with 1.5 l
  2. extractionof water and extracted with ether
  3. washThe organic layer is washed with water
  4. customdried
  5. customevaporated
  6. customthe residual oil is chromatographed on silica gel
  7. washElution with benzene
  8. customaffords 8.1 g