反应详情

Following the procedure described for Preparation 7(A), 2-(4-ethoxy-2-oxo-2,3-dihydro-benzo[b][1,4]diazepin-1-yl)-N-isopropyl-N-phenyl-acetamide (Preparation 5(B) (200 mg, 0.527 mmol) is reacted with 2-fluorobenzhydrazide (81 mg, 0.527 mmol). Purification by medium pressure chromatography eluting with a solvent gradient (CH2Cl2 to 3% MeOH in CH2Cl2) provided 180.2 mg of 2-(1-(2-fluorophenyl)-5-oxo-4,5-dihydro-2,3,6,10b-tetraaza-benzo[e]azulen-6-yl)-N-isopropyl-N-phenyl-acetamide. 1H NMR (CD2Cl2) δ 7.73 (m, 1), 7.64 (d, 1), 7.91-7.18 (m, 8), 7.12-7.00 (m, 2), 6.83 (d, 1), 4.96 (m, 1), 4.23 (d, 1), 4.06 (d, 1), 3.80 (d, 1), 3.58 (d, 1), 1.09 (d, 6); MS 470.3 (M+1)

1. customPurification by medium pressure chromatography
2. washeluting with a solvent gradient (CH2Cl2 to 3% MeOH in CH2Cl2)