反应详情

A solution of bis(2-chloroethyl)-N-(1,1-dimethylethoxy)carbonyl amine (19 g, 78 mmol) and homophthalonitrile (8.6 g, 60 mmol) and cesium carbonate (79 g, 241 mmol) was stirred at 60° C. for 12 hours. The solution cooled to room temperature and diluted with 500 ml EtOAc and washed with saturated aqueous NaHSO4 and saturated aqueous NaCl. The solution was dried over Na2SO4, concentrated in vacuo, and purified by PCTLC (30% EtOAc in Hexane) to afforded 4-cyano-N-(1,1-dimethylethloxy)carbonyl-4-(2-cyanophenyl) piperidine as a yellow/orange oil.

1. washwashed with saturated aqueous NaHSO4 and saturated aqueous NaCl
2. dry with materialThe solution was dried over Na2SO4
3. concentrationconcentrated in vacuo
4. custompurified by PCTLC (30% EtOAc in Hexane)