Trifluoroacetic acid → HCID 18997003, compound

Participants

Reaction Conditions

Reaction Steps

Trifluoroacetic anhydride (4.62 ml, 6.87 g), was added dropwise with magnetic stirring to a suspension of 9,10-dihydro-4,5-dimethoxy-9,10-dioxoanthracene-2-aldoxime (10.74 ml, 9.24 g) in pyridine (10.5 ml, 10.336 g) and dioxan (100 ml) at room temperature under nitrogen. The temperature rose from 23° C. to 31° C. The mixture was then heated at 65° C. for 2 hours. More trifluoroacetic anhydride (4.62 ml, 6.87 g) was added at 65° C. and the mixture was stirred for a further 1 hour at 65° C. More trifluoroacetic acid (1 ml, 1.487 g) was added and the mixture stirred for 16 hours at 65° C., cooled, filtered, washed with water (200 ml) and dried in vacuo at 70° C. to give the nitrile, m.p. 266°-268° C.

Provenance & Evidence