反应详情

Acetic anhydride (307 mg, 3.01 mmol) was added to a stirred mixture of t-butyl 9-amino-6,10-dioxo-1,2,3,4,7,8,9,10-octahydro-6H-pyridazino[1,2-a][1,2]diazepine-1-carboxylate (GB 2,128,984; 813.7 mg, 2.74 mmol), diisopropylethylamine (884 mg, 6.84 mmol) and CH2Cl2 (20 ml). The mixture was kept for 1 h then diluted with EtOAc, washed with NaHCO3 solution then brine, dried (MgSO4) and concentrated to yield a colourless oil. The product was purified by flash chromatography (0.5-8% MeOH/CH2Cl2) to afford 211c (804 mg, 71%) of colourless powder: mp 162°-3° C.; [α]D23 -109 (c 1.03, CH2Cl2); IR(KBr) 3358, 2974, 1733, 1693, 1668, 1528, 1462, 1431, 1406, 1371, 1278, 1271, 1250, 1233, 1217, 1154, 1124; δ1H NMR (CDCl3) δ6.32 (1H, d), 5.29-5.25 (1H, m), 4.98-4.85 (1H, m), 4.68-4.58 (1H, m), 3.55-3.39 (1H, m), 2.91-2.66 (2H, m), 2.39-2.18 (2H, m), 2.03 (3H, s), 1.88-1.64 (4H, m), 1.47 (9H, s); Anal. Calcd for C16H25N3O5 : C, 56.62; H, 7.43; N, 12.38. Found: C, 56.62; H, 7.43; N,12.36; MS (+FAB) 340 (M+ +1, 40%), 284 (100).

1. washwashed with NaHCO3 solution
2. dry with materialbrine, dried (MgSO4)
3. concentrationconcentrated
4. customto yield a colourless oil
5. customThe product was purified by flash chromatography (0.5-8% MeOH/CH2Cl2)