Acetic Anhydride → HCID 54497139, compound

Participants

Reaction Steps

46.0 g (238 mmol) of 2-amino-3-cyano-6-methyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridine in 250 ml of triethyl orthoformate were mixed with 3.5 ml of acetic anhydride and refluxed under nitrogen for 4 h. The mixture was then filtered hot under suction, and the filtrate was completely evaporated in a rotary evaporator at 80° C. The residue was taken up in 300 ml of methyl t-butyl ether and heated to boiling. After removal of the insoluble solids by filtration with suction, 45.4 g (77%) of product crystallized on stirring in an ice bath. 1.7 g (3%) of product were obtained as second fraction from the mother liquor. Melting point: 88-89° C.

Provenance & Evidence