反应详情

温度

-10 °C

2-Chloro-9-cyclopentyl-5,7,8,9-tetrahydro-6H-pyrimido[4,5-b][1,4]diazepin-6-one (0.318 g, 0.0012 mol) and MeI (0.088 mL, 0.0014 mol, 1.18 eq) were added to DMF (5 mL) and the solution cooled to −10° C. NaH (0.03 g, 0.0013 mol, 1.07 eq) was added and the RM was stirred at 0° C. for 30 min and rt for 30 min. The solvent was evaporated under reduced pressure and the product extracted using EtOAc/H2O. The organic extracts were combined, washed with sat NaCl, dried (MgSO4) and evaporated under reduced pressure to give the product as a purple oily residue (0.25 g, 75%); 1H (DMSO-d6): δ 1.55 (4H, m, 2CH2), 1.7 (2H, m, CH2), 1.9 (2H, m, CH2), 2.63 (2H, t, J=5 Hz, CH2), 3.17 (3H, s, CH3), 3.65 (2H, t, J=5 Hz, CH2), 4.74 (1H, m, CH), 8.14 (1H, s, CH); MS+ve: 281.2; Rt=3.11 min (Analytical—1).

1. customThe solvent was evaporated under reduced pressure
2. extractionthe product extracted
3. washwashed with sat NaCl
4. dry with materialdried (MgSO4)
5. customevaporated under reduced pressure