反应详情

温度

57.5 °C

A 250 mL three-necked flask was charged with a hydrochloride salt of compound 1 having 1.52 equivalents of chlorine per mole of compound 1 (6.1 g, 12 mmol) and 1:1 isopropanol:water (98 mL). The mixture was heated to 50-65° C. to dissolve the solid and the solution was stirred at 50-60° C. Isopropanol (98 mL) was slowly added over 30 min at 50-60° C. and the solution was cooled to room temperature over 3 h. Isopropanol (98 mL) was slowly added over 30 min and the solution was stirred at room temperature for 7 h. The crystals were isolated by filtration, washed with isopropanol (30 mL) and dried under vacuum for 16 h to yield the monohydrochloride salt of compound 1 (3.8 g, 8.0 mmol, 67% yield, 99.7% purity by HPLC)

1. dissolutionto dissolve the solid
2. temperaturethe solution was cooled to room temperature over 3 h
3. stirringthe solution was stirred at room temperature for 7 h
4. customThe crystals were isolated by filtration
5. washwashed with isopropanol (30 mL)
6. customdried under vacuum for 16 h