1-Piperazinecarboxylic acid, ethyl ester → HCID 12271976, compound

Participants

Reaction Steps

A mixture of 7,8,10-trichloro-10,11-dihydrodibenzo(b,f)thiepine (the preparation of which is described in Example 8) (9.5 g) and 1-ethoxycarbonylpiperazine (11.9 g) was heated to 110°-120° C. for 4 hours. The preparation of the reaction mixture is analogous to that used in the preparation of the final base in Example 8 and yields 10.8 g (82%) of an oily base which was dissolved in ethanol and neutralized with maleic acid. Addition of either precipitates the maleate, C25H26Cl2N2O6S which is crystallized from a ten-fold amount of ethanol and melts at 184°-186° C.

Provenance & Evidence