2,2,2-Trichloroethyl chloroformate → HCID 54468070, compound

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Reaction Steps

2-Cyano-6,11-dihydro-11-(3-dimethylaminopropylidene)-5H-pyrrolo[2,1-b][3]benzazepine (5 g., 17.2 mmoles) and 2,2,2-trichloroethylchloroformate (4 g., 18.8 mmoles) in 100 ml. benzene were refluxed for 18 hours. The mixture was poured onto water, washed with dilute hydrochloric acid and then with water, dried over sodium sulfate and concentrated under vacuum to yield 7.1 g. of dark red oil. It was adsorbed on 250 g. silica gel and eluted with 2 liters benzene. The eluate was discarded.

Provenance & Evidence