1-Piperazinecarboxylic acid, ethyl ester → HCID 27267238, compound

Participants

Reaction Steps

A mixture of 95.9 g (0.49 moles) of 2,6-dichlorobenzyl chloride, 77.6 g (0.49 moles) of ethyl N-piperazinocarboxylate, 500 ml of isopropyl alcohol and 70 ml of 10N sodium hydroxide was heated at reflux for 18 hours. The solution was evaporated in vacuo and gave a crystalline residue. The residue in 100 ml of water was extracted twice with 200 ml portions of dichloromethane. The combined organic extract was dried over anhydrous sodium sulfate, filtered, evaporated in vacuo and gave an oil. The oil was subjected to Kugelrohr distillation, bp 117° C./0.45 mm of mercury and gave 136.4 g of 4-(2,6-dichlorobenzyl)-1-piperazinecarboxylic acid, ethyl ester as an oil.

Provenance & Evidence