Dimethylformamide → HCID 19864322, compound

Participants

Reaction Steps

Phosphorous oxychloride (4.6 ml) was added dropwise to a stirred solution of 6-methyl-8-phenyl-5,6,7,8-tetrahydro-4H-thieno[2,3-d]azepine (3.98 g) in dimethylformamide (17 ml) cooled in an ice bath. The mixture was heated to 60° for 18 hours and then evaporated. The residue was dissolved in iced water (50 ml), basified with 2M sodium hydroxide to pH~12 and extracted with dichloromethane (2×100 ml). The extracts were dried, filtered and evaporated to a brown oil. Crystallisation from hexane gave the title product as yellow crystals (m.p. 88°).

Provenance & Evidence