Benzene → HCID 21883250, compound

Participants

Reaction Steps

A mixture of the ketol II (285 g., 1.00 mole), pyrrolidine (213 g., 3.0 mole), acetic acid (180 g., 3.0 mole) and benzene (2l) was refluxed with water separation (Dean-Stark trap) under nitrogen for 30 hours. A buffer solution of sodium acetate (285 g) in water (670 ml) and acetic acid (560 ml) was added and refluxing was continued for 24 hours. The mixture was cooled, washed with 3N sulphuric acid (2 × 500 ml) and work up to give the crude enone III (orange gum). A sample crystallized from methanol as pale yellow prisms; m.p. 133°-134° C.

Provenance & Evidence