Hydrazinecarboxylic acid, ethyl ester → HCID 21525513, compound

Participants

Reaction Steps

A mixture of 6,11-dihydro-11-[(dimethylamino)acetyl]-5H-pyrido[2,3-b][1,5]benzodiazepin-5-thione (0.12 mole) and ethyl carbazate (1.2 mole) is heated in an oil bath preheated to 195°-205° C. using a take-off condenser (45 ml. is removed). The resulting solid is mixed with methylene chloride-water and the suspension is filtered. The filtrate is separated into layers, and the organic layer is washed with water, then brine solution and dried over anhydrous magnesium sulfate. The solvent is then evaporated and the resulting residue is repeatedly crystallized from methylene chloride to give 2,9-dihydro-9-[(dimethyl-amino)acetyl]-3H-pyrido[3,2-c]-s-triazolo[4,3-a][1,5]-benzodiazepin-3-one.

Provenance & Evidence