反应详情

To a solution of 2-(6-methyl-pyridin-2-yl)-4-(5-trimethylsilanylethynyl-pyridin-3-yl)-7H-pyrrolo[2,3-d]pyrimidine (Intermediate 216) (1 eq, 0.181 mmol, 70 mg) in THF (2 ml) is added TBAF (1 M in THF, 2 eq, 0.36 mmol, 0.36 ml). The resulting mixture is stirred for 10 min at r.t., then the solvent is removed in vacuo. Water is added, then the mixture is extracted with EtOAc. The organic layer is washed with sat. aqueous NaCl solution, dried with MgSO4, and concentrated under reduced pressure. The crude product is recrystallized from EtOAc giving the title compound; [M+H]+=312; 1H-NMR (400 MHz, CDCl3): δ 12.90 (s, 1H), 9.47 (d, 1H), 8.86 (d, 1H), 8.70-8.64 (m, 2H), 7.84 (t, 1H), 7.45 (m, 1H), 7.33 (d, 1H), 6.84 (d, 1H), 3.22 (s, 1H), 2.74 (s, 3H).

1. customthe solvent is removed in vacuo
2. additionWater is added
3. extractionthe mixture is extracted with EtOAc
4. washThe organic layer is washed with sat. aqueous NaCl solution
5. dry with materialdried with MgSO4
6. concentrationconcentrated under reduced pressure
7. customThe crude product is recrystallized from EtOAc giving the title compound