反应详情

温度

95 °C

Sodium hydride (120 mg, of a 60% dispersion in mineral oil) was added to a solution of 4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidine (906 mg) and dimethylformamide (30 ml) with stirring under nitrogen. The mixture was stirred for 30 minutes and then a solution of 3-(tosyloxy) tetrahydrofuran (750 mg) in dimethyl formamide (10 ml) was added with stirring. The mixture was stirred and heated at 95° C. for 18 hours and then evaporated under vacuum. The residue was partitioned between ethyl acetate and water. The ethyl acetate layer was separated, dried and evaporated to give a residual gummy solid which was triturated with ether and filtered to give 5-(4-phenoxyphenyl)-7-(3-tetrahydrofuryl)-7H-pyrrolo[2,3-d]pyrimidin-4-ylamine m.p. 196-196.5° C.

1. stirringThe mixture was stirred for 30 minutes
2. stirringwith stirring
3. stirringThe mixture was stirred
4. customevaporated under vacuum
5. customThe residue was partitioned between ethyl acetate and water
6. customThe ethyl acetate layer was separated
7. customdried
8. customevaporated
9. customto give a residual gummy solid which
10. customwas triturated with ether
11. filtrationfiltered