反应详情

温度

80 °C

To a 250 mL three-neck round bottom flask equipped with an overhead stirrer, nitrogen inlet, and thermocouple was charged 50 mL of dry N,N-dimethylacetamide followed by 5.0 g of 7H-pyrrolo[2,3-d]pyrimidin-4-ylamine (3-1) [J. Davoll, J. Chem. Soc., 131-138 (1960)] and 11.6 g of phthalic anhydride. The resulting mixture was heated to 80° C. for 8 h and then cooled to 10° C. Water (40 mL) was added while maintaining the temperature below 15° C. The resulting slurry was aged for 4 h, then filtered, and the filter washed with 20 mL of 1:1 (v/v) dimethylacetamide/water followed by 30 mL of water. The cake was sucked dry, then washed with 50 mL of ethyl acetate. The solid was dried at 40° C. under vacuum with a nitrogen sweep to give 8.1 g of 4-phthalimido-7H-pyrrolo[2,3-d]pyrimidine (3-2); m.p. 276-277° C.

1. customTo a 250 mL three-neck round bottom flask equipped with an overhead stirrer, nitrogen inlet
2. temperaturecooled to 10° C
3. temperaturewhile maintaining the temperature below 15° C
4. filtrationfiltered
5. washthe filter washed with 20 mL of 1:1 (v/v) dimethylacetamide/water
6. customThe cake was sucked dry
7. washwashed with 50 mL of ethyl acetate
8. customThe solid was dried at 40° C. under vacuum with a nitrogen sweep