6,11-dihydrobenzo[c][1]benzothiepin-11-amine

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 8.8 g of 11-amino-6,11-dihydrodibenzo[b,e]thiepin, 6.0 g of 5-chlorovaleryl chloride and 100 ml of dioxane is heated with stirring under reflux for 15 hours. The solvent is distilled off under reduced pressure. The residue is recrystallized from ethanol to give 12.5 g of the title compound, m.p. 155°-156° C. is heated under reflux for 15 hours The solvent is distilled off under reduced pressure The residue is recrystallized from ethanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2.3 g of 11-amino-6,11-dihydrodibenzo[b,e]thiepin, 2.9 g of 4-[4-(4-fluorophenyl)-1-piperazinyl]butyric acid, 2.3 g of dicyclohexylcarbodiimide and 50 ml of methylene chloride is stirred at room temperature for 15 hours. After removal of the precipitated crystals by filtration, the filtrate is concentrated under reduced pressure. The residue is recrystallized from chloroform-n-hexane to give 1.9 g of the title compound, m.p. 194°-194.5° C.; After removal of the precipitated crystals by filtration the filtrate is concentrated under reduced pressure The residue is recrystallized from chloroform-n-hexane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 8.8 g of 11-amino-6,11-dihydrodibenzo[b,e]thiepin, 6.0 g of 5-chlorovaleryl chloride and 100 ml of dioxane is heated with stirring under reflux for 15 hours. The solvent is distilled off under reduced pressure. The residue is recrystallized from ethanol to give 12.5 g of the title compound, m.p. 155°-156° C. is heated under reflux for 15 hours The solvent is distilled off under reduced pressure The residue is recrystallized from ethanol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2.3 g of 11-amino-6,11-dihydrodibenzo[b,e]thiepin, 2.9 g of 4-[4-(4-fluorophenyl)-1-piperazinyl]butyric acid, 2.3 g of dicyclohexylcarbodiimide and 50 ml of methylene chloride is stirred at room temperature for 15 hours. After removal of the precipitated crystals by filtration, the filtrate is concentrated under reduced pressure. The residue is recrystallized from chloroform-n-hexane to give 1.9 g of the title compound, m.p. 194°-194.5° C.; After removal of the precipitated crystals by filtration the filtrate is concentrated under reduced pressure The residue is recrystallized from chloroform-n-hexane