反应详情

As illustrated in the scheme above and following General Procedure 2, 3-amino-7-chloro-5-(2,4-dimethoxy-5-pyrimidinyl)-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one (1.15 g, 3.18 mmol) and thiophosgene (0.49 mL, 6.4 mmol) were combined. Purification of the crude product by silica gel column chromatography (9:1 CH2Cl2:EtOAc) provided the title compound as a viscous dark yellow oil (0.560 g, 44%). 1H-NMR (CDCl3): δ 8.60 (s, 1H), 7.55 (dd, J=2.5 Hz, J=8.8 Hz, 1H), 7.33 (d, J=8.8 Hz, 1H), 7.17 (d, J=2.5 Hz, 1H), 5.16 (s, 1H), 4.07 (s, 3H), 3.78 (s, 3H), 3.49 (s, 3H). MS (ESI) (M+H)+=404.

1. customPurification of the crude product by silica gel column chromatography (9:1 CH2Cl2:EtOAc)