HRID2369349

反应详情

EQUATION

反应方程式

HRID 2369349 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe oil was precipitated when 2 mL of heptane
  2. additionwas added
  3. dissolutionAccordingly, the oily substance was dissolved by ultrasonic treatment
  4. customto prepare a clear solution
  5. additionwere added
  6. stirringby stirring at room temperature
  7. stirringStirring for about one hour
  8. customresulted in gelation and subsequent precipitation of a solid
  9. stirringFurther, stirring
  10. customA part of the suspension (2 mL) was separated
  11. filtrationthe solid was collected by filtration through a glass
  12. filtrationfilter
  13. customThe solid was dried under reduced pressure at room temperature