反应详情

温度

5 °C

In a 250 mL flask a hydrochloride salt of compound 1 having 1.52 equivalents of chlorine per mole of compound 1 (5.0 g, 9.8 mmol) was suspended in 1:1 isopropanol:water (79 mL). The slurry was heated in a stepwise fashion, from 50° C. to 70° C. in 5° C. increments, to dissolve the solid. The solution was allowed to cool and isopropanol (80 mL) was added in one portion. Additional isopropanol (80 mL) was added dropwise and crystal formation was observed after about 75 mL was added. The slurry was stirred at room temperature for 16 h. The crystals were isolated by filtration, washed with cold 85% isopropanol/water (10 mL) followed by isopropanol (10 mL) and dried under vacuum to yield the monohydrochloride salt of compound 1.

1. dissolutionto dissolve the solid
2. temperatureto cool
3. additionwas added
4. customThe crystals were isolated by filtration
5. washwashed with cold 85% isopropanol/water (10 mL)
6. customdried under vacuum