Originator
Clofekton,Yoshitomi,Japan,1974
Manufacturing Process
A mixture of 5.0 g of 3-chloro-5-(3-chloropropyl)-10,11-dihydro-5Hdibenz[b,f]azepine, 5.0 g of 4-carbamoyl-4-piperidinopiperidine and 50 ml of
dimethylformamide is heated at 100°C for 10 hours. The solvent is distilled
off. After the addition of a 2% sodium carbonate solution to the flask, the
content is scratched to yield a semisolid, which is dissolved in 50 ml of
isopropanol. A solution of 5 g of maleic acid in 50 ml of isopropanol is added,
and the precipitate is collected by filtration and recrystallized from isopropanol
to give 5.6 g of crystalline 3-chloro-5-[3-(4-carbamoyl-4-piperidinopiperidino)
propyl]-10,11-dihydro-5H-dibenz[b,f]azepine di(hydrogen maleate) with 1/2
molecule of water of crystallization melting at 181°C to 183°C.
