反应详情

As illustrated in the scheme above and following General Procedure 6, KHMDS (7.0 mL of 0.5 M in toluene, 3.5 mmol), 7-chloro-5-(2,4-dimethoxy-5-pyrimidinyl)-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one (1.16 g, 3.35 mmol), trisyl azide (2.60 g, 8.40 mmol) and acetic acid (0.85 mL, 14.8 mmol) were combined. After workup, purification of the crude product by silica gel column chromatography (2:3 hexanes:EtOAc) provided the title compound as a pale yellow solid (1.23 g, 95%). 1H-NMR (CDCl3): δ 8.64 (s, 1H), 7.54 (dd, J=2.3 Hz, J=8.8 Hz, 1H), 7.33 (d, J=8.8 Hz, 1H), 7.19 (d, J=2.3 Hz, 1H), 4.51 (s, 1H), 4.08 (s, 3H), 3.78 (s, 3H), 3.47 (s, 3H). MS (ESI) (M+H)+388.

1. customAfter workup, purification of the crude product by silica gel column chromatography (2:3 hexanes:EtOAc)