反应详情

To a suspension of (6-aminopyrimidin-4-yl)methanol (52 mg, 0.42 mmole) in CH2Cl2 (2 mL) was added DMF (0.03 mL, 0.42 mmole) then POCl3 (0.04 mL, 0.42 mmole) at room temperature. After 2 hours, Et3N (0.3 mL) was added and stirring continued. After 18 hours, the mixture was concentrated. The residue was taken up in saturated NaHCO3 and extracted with CH2Cl2 (4×). The combined organic layers were dried (MgSO4), filtered, and concentrated to give the title compound as its DMF amidine. 1H-NMR (300 MHz, d6-DMSO) δ 8.78 (s, 1H), 8.65 (s, 1H), 6.90 (s, 1H), 4.60 (s, 2H), 3.18 (s, 3H), 3.05 (s, 3H).

1. customat room temperature
2. waitAfter 18 hours
3. concentrationthe mixture was concentrated
4. extractionextracted with CH2Cl2 (4×)
5. dry with materialThe combined organic layers were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated