反应详情

11-piperazinyl-dibenzo[b,f][1,4]thiazepine hydrochloride (40 g) obtained in step c), sodium carbonate (69.3 g), sodium iodide (0.65 g), and 2-chloroethoxyethanol (14.7 g) were added to a solution of n-propyl alcohol (260 ml) and N-methylpyrrolidone (65 ml), and reflux was conducted for 24 hours. Ethyl acetate (327 ml) was added thereto, washing was conducted using water (2×1000 ml), an organic layer was separated to be dried with magnesium sulfate, and a solvent was removed at reduced pressure, thereby oil was created. The resulting oil was completely dissolved in ethanol, and fumaric acid (7.1 g) was added thereto, to produce 11-[4-[2-(hydroxyethoxy)ethyl]-1-piperazinyl]-dibenzo[b,f][1,4]thiazepine fumarate (34 g).

1. temperaturereflux
2. washwashing
3. customan organic layer was separated
4. dry with materialto be dried with magnesium sulfate
5. customa solvent was removed at reduced pressure
6. dissolutionThe resulting oil was completely dissolved in ethanol
7. additionfumaric acid (7.1 g) was added