反应详情

Phenylmaleic anhydride (20 g, 115 mmol), sodium acetate trihydrate (1875 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 1 h. 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) δ 3.43 (2H, broad peak), 7.17 (1H, s), 7.44 (3H, m), 7.81 (2H, m); MS (ES+) m/e 189 [MH+].

1. temperatureat reflux for 15 h
2. temperatureto cool
3. waitThe reaction mixture was left
4. temperatureto cool in the fridge for 1 h
5. customThe solid produced
6. filtrationwas filtered
7. washwashed with water and diethyl ether
8. custombefore drying in a vacuum oven at 40° C.