Acetonitrile → HCID 54001000, compound

Participants

Reaction Steps

4.715 g (9.7 millimol) of 3-chloro-4-[[4-[4-(diethylamino)-butyl]-1-piperidinyl]acetyl ]-1-methyl-1,4,9,10-tetrahydropyr rolo[3,2-b][1,5]benzodiazepin- 10-one were dissolved in a mixture of 5 ml of 85% formic acid and 25 ml of dimethylformamide and after the addition of 0.5 g of 10% palladium/activated charcoal the mixture was refluxed for 3 hours. 7.0 ml of formic acid were added, the mixture was refluxed for a further 6 hours and then, after the addition of a further 4.0 ml of formic acid and 0.8 g of 10% palladium/activated charcoal, the mixture was finally refluxed for a further 8 hours. The mixture was filtered while hot, the filtrate was evaporated down in vacuo and the residue was purified by column chromatography (silica gel; dichloromethane/ethyl acetate/methanol/conc. ammonia 3.5:1.5:0.46:0.06 v/v). 1.45 g (33% of theory) of colourless crystals were obtained, m.p. 196°-198° C. (acetonitrile), which were found according to thin layer chromatography and IR, UV and 1H-NMR spectra, to be identical to a preparation obtained according to Example 39.

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