反应详情

温度

2 °C

A flask was charged with crude N-[4-[2-(2-amino-4,7-dihydro-4-oxo-1H-pyrrolo[2,3-d]pyrimidin-5-yl)ethyl]benzoyl]-L-glutamic acid (4 g), water (28 ml) and NaOH (3 equivalents) at 25° C. Complete dissolution was obtained. The pH was corrected to 10.0 with HCl 1M and acetone (120 mL) was added drop wise over a period of 50 min. The obtained suspension was cooled to 2° C. in one hour, stirred at 2° C. for 10 hours and filtered. The solid was washed with acetone (30 mL) and dried at 40° C. under vacuum (18 mbar) for about 16 hours affording the title compound.

1. dissolutionComplete dissolution
2. customwas obtained
3. additionwas added drop wise over a period of 50 min
4. filtrationfiltered
5. washThe solid was washed with acetone (30 mL)
6. customdried at 40° C. under vacuum (18 mbar) for about 16 hours