反应详情

A mixture of 17.0 g. (0.15 mole) of 1-ethyl-3,4-epoxypyrrolidine, 20.5 g. (0.16 mole) of o-chlorophenol and 3 drops concentrated hydrochloric acid was heated on a steam both overnight. The oil was dissolved in methylene chloride and washed with three 50-ml. portions of 5% sodium hydroxide and one 50-ml. portion of water. The methylene chloride solution was dried over anhydrous sodium sulfate, concentrated and chromatographed on silica gel to give 8.9 g. (25%) of an oil as residue. The oil was converted to the hydrochloride and recrystallized from ethyl acetate-acetonitrile to yield white powder, m.p. 108°-110° C.

1. additionA mixture of 17.0 g
2. washwashed with three 50-ml
3. dry with materialThe methylene chloride solution was dried over anhydrous sodium sulfate
4. concentrationconcentrated
5. customchromatographed on silica gel
6. customto give 8.9 g
7. customrecrystallized from ethyl acetate-acetonitrile
8. customto yield white powder, m.p. 108°-110° C.