反应 #1365743

反应方程式

Phenylmaleic anhydride

sodium acetate trihydrate

hydrazine monohydrate

→

required product

收率 33.9%

4-Phenylpyridazine-3.6-dione

收率 33.9%

溶剂

acetic acid

反应条件

后处理

1. 1
   温度at reflux for 15 h
2. 2
   温度to cool
3. 3
   workup.WAITThe reaction mixture was left
4. 4
   温度to cool in the fridge for 1h
5. 5
   其他The solid produced
6. 6
   过滤was filtered
7. 7
   洗涤washed with water and diethyl ether
8. 8
   其他before drying in a vacuum oven at 40° C.

实验过程

Phenylmaleic anhydride (20 g, 115 mmol), sodium acetate trihydrate (18.75 g, 138 mmol), hydrazine monohydrate (6.68 ml, 133 mmol) and 40% aqueous acetic acid (400 ml) were heated at reflux for 15 h then allowed to cool. The reaction mixture was left to cool in the fridge for 1h. The solid produced was filtered and washed with water and diethyl ether before drying in a vacuum oven at 40° C. to give the required product (7.26 g). 1H NMR (250 MHz, DMSO) 8 3.43 (2H, broad peak), 7.17 (1H, s), 7.44 (3H, m), 7.81 (2H, m); MS (ES+) m/e 189 [MH+].

来源