反应 #586170

反应方程式

1,3-Dimethyl-4-nitro-1H-pyrazol-5-yl-hydrazine

7,8-dimethoxy-1H-[1]benzazepin-2,5(3H, 4H)-dione

water

→

title compound

收率 12.2%

5-[(1,3-Dimethyl-4-nitro-1H-pyrazol-5-yl)hydrazono]-7,8-dimethoxy-1,3,4,5-tetrahydro-benzo[b]azepin-2-one

收率 12.2%

溶剂

acetic acid

反应条件

后处理

1. 1
   温度cooled
2. 2
   过滤The precipitate was then filtered off

实验过程

1,3-Dimethyl-4-nitro-1H-pyrazol-5-yl-hydrazine (0.073 g, 0.4 mmol) was added to a suspension of 7,8-dimethoxy-1H-[1]benzazepin-2,5(3H, 4H)-dione (0.100 g, 0.4 mmol) in acetic acid (5 ml) with stirring under argon. The mixture was heated at 70° C. for 2 days, cooled and water (5 ml) added. The precipitate was then filtered off to give the title compound as a yellow solid (0.019 g, yield 11.5%); 1H-NMR (DMSO-d6, 300 MHz): δ (ppm)=12.8 (v br s; 1 H), 9.59 (s; 1H), 7.2 (s; 1H), 6.63 (s; 1H), 3.96 (s; 3H), 3.75-3.77 (s, 6H), 3.05 (br t, 2H), 2.57 (br t, 2H), 2.35 (s, 3H).

来源