HRID1744162
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
To a solution of tert-butyl 4-[3′-(2-{[(cyanomethyl)amino]carbonyl}-1-piperidinyl)[1,1′-biphenyl]-4-yl]-1-piperazinecarboxylate (249 mg, 0.51 mmol) in dioxane (5 mL) was added methanesulfonic acid (0.1 mL, 1.5 mmol). The mixture was stirred overnight, then partitioned between EtOAc and 1 M NaOH. The organic phase was washed with brine and dried over MgSO4. Purification by flash chromatography (5% MeOH/dichloromethane with 0.5% NH4OH) gave N-(cyanomethyl)-1-[4′-(1-piperazinyl)[1,1′-biphenyl]-3-yl]-2-piperidinecarboxamide.
WORKUP
后处理
- custompartitioned between EtOAc and 1 M NaOH
- washThe organic phase was washed with brine
- dry with materialdried over MgSO4
- customPurification by flash chromatography (5% MeOH/dichloromethane with 0.5% NH4OH)