Triethylamine → HCID 86734517, compound

Participants

Reaction Steps

To a solution of 12.0 g of 1-chlorocarbonyl-5-o-chlorophenyl-7-ethyl-2,3-dihydro-1H-thieno[2,3-e][1,4]diazepine and 3.8 g of triethylamine in 50 ml of toluene is added dropwise a solution of 3.8 g of N-methylpiperazine in 10 ml of toluene with stirring. The whole solution is refluxed with stirring for 30 minutes, and then cooled. The precipitated triethylamine hydrochloride is filtered off. After the filtrate is washed with water and dried over anhydrous magnesium sulfate, the solvent is evaporated under reduced pressure. The residue is treated with ethanolic hydrogen chloride to give 5-o-chlorophenyl-7-ethyl-1-(4-methyl-1-piperazinylcarbonyl)-2,3-dihydro-1H-thieno[2,3-e][1,4]diazepine dihydrochloride 1/2 -hydrate as yellow crystals. This product, when recrystallized from acetone containing water, melts at 248°-250° C with decomposition.

Provenance & Evidence