HRID1989867

反应详情

EQUATION

反应方程式

HRID 1989867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of intermediate (23) (0.0014 mol) in concentrated HCl (25 ml) and dioxane (20 ml) was stirred and refluxed for 4 hours, cooled and poured out into water. The mixture was extracted with DCM. The organic layer was separated, dried, filtered and the solvent was evaporated. The residue was triturated in DIPE. The precipitate was filtered off and dried, yielding 0.48 g of α-phenyl-1-[4-[[[4′-(trifluoromethyl)[1,1′-biphenyl]-2-yl]carbonyl]amino]phenyl]-4-piperidineacetic acid monohydrochloride (intermediate 24, mp. 196° C.).

WORKUP

后处理

  1. temperaturerefluxed for 4 hours
  2. temperaturecooled
  3. extractionThe mixture was extracted with DCM
  4. customThe organic layer was separated
  5. customdried
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customThe residue was triturated in DIPE
  9. filtrationThe precipitate was filtered off
  10. customdried