Acetic Anhydride → HCID 54497139, compound

Participants

Reaction Steps

3.5 ml of acetic anhydride were added to 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 and the mixture was boiled under nitrogen and at reflux for 4 h. After that, the mixture was filtered off with suction, in the hot, through a suction filter and the filtrate was evaporated right down at 80° C. on a rotary evaporator. The residue was taken up in 300 ml of methyl t-butyl ether and this mixture was heated to boiling. After the insoluble solids had been filtered off with suction, 45.4 g (77%) of the product crystallized out in an icebath with stirring. A further 1.7 g (3%) of product were obtained from the mother liquor as a second fraction. m.p.: 88-89° C.

Provenance & Evidence