HRID372172
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureto reflux
- customFor purification
- extractionthe benzene extract
- customis chromatographed on silica gel (0.2-0.5 mm) with chloroform
- 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