1-(2-Hydroxyethyl)piperazine → HCID 12271968, compound

Participants

Reaction Steps

A mixture of 7,8-difluoro-10-chloro-10,11-dihydrodibenzo(b,f)thiepine (see Example 15) (6.35 g), 1-(2-hydroxyethyl)-piperazine (6.1 g) and chloroform (10 ml) was refluxed for 7.5 hours under stirring. The chloroform was evaporated under diminished pressure, the residue dissolved in benzene (200 ml) and the solution thoroughly washed with water and shaken with 3 N-HCl (150 ml). The precipitated hydrochloride was filtered, added to the aqueous layer of the filtrate and the resultant suspension made alkaline by addition of ammonium hydroxide. The liberated base was taken up in benzene and the extract yielded 7.1 g (84%) of the desired oily base. This was crystallized from aqueous acetone in the form of the hemihydrate, which in the pure state melts at 101°-102° C.

Provenance & Evidence