Sodium Acetate → HCID 13101160, compound

Participants

Reaction Steps

3.0 g of Pd/C (10%) and 15.0 g (183 millimoles) of finely powedered sodium acetate were added to 19.2 g (63.2 millimoles) of 1,3-dichloro-4,5-dihydrodithieno[3,4-b:3',4'-e]azepine-5,9-dione in 600 ml of 1-methylpyrrolid-2-one, and hydrogenation was carried out in a 2.5 l Rollhofer apparatus for 5 hours under a hydrogen pressure of 200 bar and at 80° C. Thereafter, the mixture was filtered under suction, the residue was washed with pyrrolidone and then H2O, the filtrate was poured onto 5 l of ice water, acidified with concentrated HCl and stirred for a further hour, after which the solid was filtered off under suction with thorough washing with H2O, and the crude product was dried. The yield was 12.6 g (85%) and the melting point 267°-270° C.

Provenance & Evidence