反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
(8S)-2-{(E)-2-[6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridin-2-yl]vinyl}-8-(2-trifluoromethylphenyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyridine (810.18 mg) was dissolved in 8 mL of a D-tartaric acid-ethanol solution (751.13 mg/10 mL) with stirring at room temperature. The oil was precipitated when 2 mL of heptane was added. Accordingly, the oily substance was dissolved by ultrasonic treatment to prepare a clear solution. Several mg of crystals of the 1.5 D-tartrate prepared according to Example 1 were added, followed by stirring at room temperature. Stirring for about one hour resulted in gelation and subsequent precipitation of a solid. Further, stirring was continued while gradually adding 14 mL of heptane. A part of the suspension (2 mL) was separated and the solid was collected by filtration through a glass filter. The solid was dried under reduced pressure at room temperature to obtain 71.14 mg of the title compound as white solid crystals.
WORKUP
后处理
- customThe oil was precipitated when 2 mL of heptane
- additionwas added
- dissolutionAccordingly, the oily substance was dissolved by ultrasonic treatment
- customto prepare a clear solution
- additionwere added
- stirringby stirring at room temperature
- stirringStirring for about one hour
- customresulted in gelation and subsequent precipitation of a solid
- stirringFurther, stirring
- customA part of the suspension (2 mL) was separated
- filtrationthe solid was collected by filtration through a glass
- filtrationfilter
- customThe solid was dried under reduced pressure at room temperature