Ethyl chloroformate → HCID 20474131, compound

Participants

Reaction Steps

Into a 50 ml round bottomed flask equipped with an efficient condenser sealed with a calcium chloride tube were placed 10 ml of ethylchloroformate and 1 g of 2-(4'-chlorobenzyl)-hexahydro-1,2,4-triazine-3,5-dione. The mixture was refluxed for 3 hours, the solvent was removed in vacuum and ice water was added cautiously to the residue. The solution was adjusted to a neutral pH with a saturated solution of sodium bicarbonate. The crystals thus formed were filtered off by suction and recrystallized from isopropanol to yield 0.8 g (50%) of 1-ethoxycarbonyl-2-(4'-chlorobenzyl)-hexahydro-1,2,4-triazine-3,5-dione; m.p. 135°.

Provenance & Evidence