HRID12958
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
A solution of 3.45 g of L-tartaric acid (1.07 eq.) in 56 g of water was added to a flask containing a slurry of 8.00 g of the product of Example 41G in anhydrous ethanol (44 g). The mixture was heated under reflux and after 30 minutes most solids had dissolved. The mixture was cooled at 5° C. per hour to 60° C., and then allowed to cool to ambient temperature overnight. After cooling the mixture to −15° C. the product slurry was filtered and dried at 45-50° C. overnight to provide the title compound (10.64 g, 94.8%).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux and after 30 minutes most solids
- dissolutionhad dissolved
- temperatureThe mixture was cooled at 5° C. per hour to 60° C.
- temperatureAfter cooling the mixture to −15° C. the product slurry
- filtrationwas filtered
- customdried at 45-50° C. overnight