Piperidine → HCID 21442752, compound

Participants

Reaction Steps

To a mixture of 178 mg. of 7,8-dimethyl-6-phenyl-4H-thieno[3,2-f]-s-triazolo[1,5-a][1,4]diazepine-2-carboxylic acid 5-oxide, 0.1 ml. of triethylamine and 5 ml. of tetrahydrofuran is added 0.07 ml. of ethyl chlorocarbonate under stirring and cooling on an ice-sodium chloride bath, and the mixture is stirred for 5 minutes. Then, to the mixture is added 0.07 ml. of piperidine, followed by stirring for 30 minutes, and water is added to the resulting mixture. Then, the mixture is extracted with ethyl acetate. The ethyl acetate layer is washed with water, dried over sodium sulfate and then the solvent is evaporated. Thereafter, addition of ether to the residue gives 7,8-dimethyl-6-phenyl-2-piperidinocarbonyl-4H-thieno[3,2-f]-s-triazolo[1,5-a][1,4]diazepine-5-oxide as crystals. Recrystallization from ethyl acetate gives colorless prisms melting at 213° to 214° C.

Provenance & Evidence