反应详情

温度

0 °C

A stirred solution of 1-[(4-nitrophenyl)sulfonyl]-4-[2-(1-piperidinyl)ethoxy]1H-indazole (0.39 g, 0.91 mol) in methanol is treated with Raney Nickel followed by hydrazine (0.2 ml, 6.3 mmol), stirred at 0° C. for 2 hr and decanted. The catalyst is washed with a methanol: methylene chloride 3:7 mixture. The washes and supernatant are combined and concentrated in vacuo. The resultant residue is purified by flash chromatography (silicagel, EtOAc/2M NH3 in methanol 8:2) to give the title product as a white solid, 0.15 g, mp 149-150° C. (dec), identified by NMR and mass spectral analyses.

1. customdecanted
2. washThe catalyst is washed with a methanol: methylene chloride 3:7 mixture
3. concentrationconcentrated in vacuo
4. customThe resultant residue is purified by flash chromatography (silicagel, EtOAc/2M NH3 in methanol 8:2)