反応 #959454

反応方程式

1-(cyclobutylmethyl)-5-nitro-1H-benzotriazole

→

1-(cyclobutylmethyl)-1H-benzotriazol-5-amine

溶媒

ethanol

反応条件

後処理

1. 1
   ろ過The catalyst was filtered onto a pad of diatomaceous earth
2. 2
   洗浄washed with ethanol (100 mL)
3. 3
   濃縮The filtrate was concentrated

実験手順

A mixture of 1-(cyclobutylmethyl)-5-nitro-1H-benzotriazole (3-2, 1.2 g, 5.17 mmol, 1 equiv) and 10% palladium on carbon (0.6 g) in ethanol (50 mL) was stirred at 23° C. under a hydrogen balloon for 20 h. The catalyst was filtered onto a pad of diatomaceous earth and washed with ethanol (100 mL). The filtrate was concentrated to give 1-(cyclobutylmethyl)-1H-benzotriazol-5-amine (3-3) as a grey solid. 1H NMR (300 MHz, CDCl3) δ 7.32 (d, 1H, J=8.9 Hz), 7.20 (d, 1H, J=1.8 Hz), 6.92 (dd, 1H, J=8.5, 1.8 Hz), 4.56 (d, 2H, J=7.3 Hz), 3.80 (br s, 2H), 2.95 (p, 1H, J=7.3 Hz), 2.05 (m, 2H), 1.88 (m, 4H) ppm. LRMS m/z (M+H) 203.0 found, 203.1 required.

出典