反应详情

A stirred solution of 5-nitro-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole (1.00 g, 4.04 mmol) in EtOAc (10 mL) was degassed for 10 min and then placed under vacuum and filled with nitrogen. The reaction mixture was placed under vacuum again, palladium on carbon (10% wt./wt, 272 mg, 0.256 mmol) was added and the resulting mixture was stirred under an atmosphere of hydrogen at RT for 20 hr. The reaction mixture was filtered through a pad of celite and the filtrate was concentrated in vacuo to yield the title compound, Intermediate D1 as a pale yellow solid (553 mg, 2.47 mmol, 61% yield); Rt 1.38 min, Basic method, m/z 218.3 (M+H)+ (ES+); 1H NMR (400 MHz, DMSO-d6) δ: 1.52-1.58 (2H, over-lapping m), 1.71 (1H, m), 1.90 (1H, m), 2.01 (1H, m), 2.36 (1H, m), 3.68 (1H, m), 3.86 (1H, m), 4.85 (2H, s), 5.67 (1H, dd), 6.74 (1H, m), 6.81 (1H, dd), 7.40 (1H, m), 7.75 (1H, d).

1. additionfilled with nitrogen
2. filtrationThe reaction mixture was filtered through a pad of celite
3. concentrationthe filtrate was concentrated in vacuo