HRID1670840
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
Treat a mixture of 3-[4-(tert-butyl-diphenyl-silanyloxy)-cyclohexyl]-1-[3,5-dichloro-4′-(4-trifluoromethyl-piperidine-1-carbonyl)-biphenyl-4-ylmethyl]-pyrrolidin-2-one (0.18 g), THF (6 mL) and water (6 mL) with TFA (2 mL) at room temperature for 1 hour and then at 55° C. for 12 hours. Cool the reaction, dilute with ethyl acetate, and wash with sodium bicarbonate (sat.). Dry the organic layer (Na2SO4), remove the solvent in vacuo to afford crude product, and purify on silica gel column with 50% ethyl acetate in hexanes to 100% ethyl acetate gradient to afford 0.075 g (59%) of the titled product. MS (m/z): 599 (M+).
WORKUP
后处理
- additionTreat
- temperatureCool
- customthe reaction
- washwash with sodium bicarbonate (sat.)
- dry with materialDry the organic layer (Na2SO4)
- customremove the solvent in vacuo
- customto afford crude product
- custompurify on silica gel column with 50% ethyl acetate in hexanes to 100% ethyl acetate gradient