Ethanol → HCID 54321746, compound

Participants

Reaction Steps

An ethanol (3.5 l) solution of 2-cyano-3,3-bis-methylsulfanyl-acrylic acid methyl ester (454.3 g, 2.23 mol) and 2,4,6-trichlorophenylhydrazine (472.7 g, 2.23 mol) was vigorously refluxed for 1.5 hours. The reaction mixture was allowed to stand overnight at ambient temperature. Water (850 ml) was added, and the resulting mixture was briskly stirred for 30 minutes. The granular precipitate was filtered and washed with a water/ethanol(1:3 in volume)solution (1 l). The air-dried product was further dried under vacuum (45° C.) for 2 days to afford the title compound as a yellow crystalline solid, m.p. 160°-162° C.

Provenance & Evidence