反应详情

温度

45 °C

To a slurry of compound 8 (1.0 eq) in MeCN (3.0 vol) is added water (0.83 vol) followed by concentrated aqueous HCl (0.83 vol). The mixture is heated to 45±5° C. After stirring for 24 to 48 hours the reaction is complete and the mixture is allowed to cool to ambient. Water (1.33 vol) is added and the mixture stirred. The solid is collected by filtration, washed with water (2×0.3 vol), and partially dried on the filter under vacuum. The solid is dried to constant weight (<1% difference) in a vacuum oven at 60° C. with a slight N2 bleed to afford compound 9 as an off-white solid.

1. temperatureto cool to ambient
2. stirringthe mixture stirred
3. filtrationThe solid is collected by filtration
4. washwashed with water (2×0.3 vol)
5. custompartially dried on the
6. filtrationfilter under vacuum
7. dry with materialThe solid is dried to constant weight (<1% difference) in a vacuum oven at 60° C. with a slight N2