反应详情

温度

100 °C

To a solution of 11 (3.44 g, 10.0 mmol) in MeOH (40 mL) was added a saturated methanolic NH3 solution (100 mL). The solution was heated in a sealed flask at 100° C. for 30 h. The solvent was evaporated and the residue was crystallized from EtOH to give 12 (1.20 g) in 40% yield: mp 190°-193° C.; TLC Rf 0.37 (AcOEt/MeOH=1:1); UV λmax (EtOH): 260 nm (ε14 000); 1H NMR (DMSO-d6 /D2O): δ1.20-1.56 (m, 5 H, CH3 +CH2 P), 3.40-4.10 (m, 2 H, CH2OP), 4.30 (m, 2 H, CH2O), 5.60 (s, 2 H, OCH2N), 7.80, 8.12 (2 s, 2 H, HC(2) +HC(8)). Anal. (C10 H19N6O4P) C, H, N.

1. customThe solvent was evaporated
2. customthe residue was crystallized from EtOH