反应详情

温度

50 °C

To a solution (4 mL) of a free form (500 mg) of (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one in ethanol was added dropwise 2M methanesulfonic acid ethanol solution (1 mL) with stirring on an oil bath at 50° C. The bath was removed, ethyl acetate (8 mL) and seed crystals were added and the mixture was stirred to allow precipitation of crystals. After stirring under ice-cooling, the crystals were collected through filtration, washed with ethyl acetate/ethanol (2:1) and dried under reduced pressure at 50° C. for 18 hr to give the title compound (507 mg).

1. customThe bath was removed
2. additionethyl acetate (8 mL) and seed crystals were added
3. stirringthe mixture was stirred
4. customprecipitation of crystals
5. stirringAfter stirring under ice-
6. temperaturecooling
7. filtrationthe crystals were collected through filtration
8. washwashed with ethyl acetate/ethanol (2:1)
9. customdried under reduced pressure at 50° C. for 18 hr