Sodium hydride → HCID 18319530, compound

Participants

Reaction Steps

To a solution of ethyl 9-(4-chloro-1-oxobutylamino)-2,3-dihydro-1-benzoxepin-4-carboxylate (0.44 g) in N,N-dimethylformamide (4.4 ml) was added sodium hydride (0.17 g, 60%) at ambient temperature. The reaction mixture was stirred for 1.5 hours at the same temperature and partitioned between ethyl acetate and 1N hydrochloric acid. The organic layer was washed successively with water and brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was purified by medium pressure liquid chromatography (silica gel) using a mixture of ethyl acetate and n-hexane (1:4˜1:1) to give a solid of ethyl 2,3-dihydro-9-(2-oxo-1-pyrrolidinyl)-1-benzoxepin-4-carboxylate (0.21 g).

Provenance & Evidence