反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5.0 G. of the salt of racemic 3-{2-[4-(8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-oxazolidinone with (+)-(R,R)-tartaric acid [α546 =+15.0° (water; c = 10%)] in the molar ratio of 1:1 are dissolved in 500 ml. of acetone and, after stirring for 24 hours at room temperature, the mixture is filtered. The filter cake is washed with acetone, dried under reduced pressure, and there is obtained 3-[2-{4-[(R)-8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl}-1-piperazinyl]-ethyl]-2-oxazolidinone-(R,R)-tartrate (1:1); α365 =+98.6° (dimethylformamide; c = 2.0%); decomposition point 172° C. After liberation of the base by treatment with aqueous sodium hydroxide, there is obtained crystalline (R)-3-{2-[4-(8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl}-2-oxazolidinone; α365 =+183.85° (chloroform; c = 0.5%) in a purity above 99%. The yield amounts to 54.4% of theory.
WORKUP
后处理
- filtrationthe mixture is filtered
- washThe filter cake is washed with acetone
- customdried under reduced pressure