反应详情

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+].

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