HRID372172

反应详情

EQUATION

反应方程式

HRID 372172 的结构方程式

PROCEDURE

实验过程

2.3 G. of enriched (R)-1-(8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine [αD = -25.0° (chloroform; c = 2.50%)] are heated to reflux with stirring for 24 hours in 0.57-M methanesulfonic acid and worked up in a manner analogous to that described in Example 13. For purification, the benzene extract is chromatographed on silica gel (0.2-0.5 mm) with chloroform. The eluted oily racemic 8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-ol melts at 90.5° C. after recrystallization from n-hexane.

WORKUP

后处理

  1. temperatureto reflux
  2. customFor purification
  3. extractionthe benzene extract
  4. customis chromatographed on silica gel (0.2-0.5 mm) with chloroform
  5. customThe eluted oily racemic 8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-ol melts at 90.5° C. after recrystallization from n-hexane