HRID1989867
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
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
- temperaturerefluxed for 4 hours
- temperaturecooled
- extractionThe mixture was extracted with DCM
- customThe organic layer was separated
- customdried
- filtrationfiltered
- customthe solvent was evaporated
- customThe residue was triturated in DIPE
- filtrationThe precipitate was filtered off
- customdried