反应详情

温度

60 °C

To 91.0 g (0.32 mmol) of the purified trans-5-chloro-2,3,3a,12b-tetrahydro-2-methyl-1H-dibenzo[2,3;6,7]-oxepino[4,5-c]pyrrole obtained in Production Example 2 there were added 310 mL of 99.5% ethanol and 40.6 g (0.35 mol) of maleic acid, and the obtained mixture was heated to 60° C. to obtain a homogeneous solution. The solution was cooled to −10° C. over a period of 18 hours. The precipitated crystals were separated off by filtration, and the crystals were washed with 45 mL of cold ethanol and dried to obtain 108.2 g of trans-5-chloro-2,3,3a,12b-tetrahydro-2-methyl-1H-dibenzo[2,3;6,7]-oxepino[4,5-c]pyrrole maleate as a white solid. The yield was 84.6%.

1. customto obtain a homogeneous solution
2. temperatureThe solution was cooled to −10° C. over a period of 18 hours
3. customThe precipitated crystals were separated off by filtration
4. washthe crystals were washed with 45 mL of cold ethanol
5. customdried