反应详情

Semicarbazide chlorohydrate (2.22 g, 20 mmol) and sodium acetate (1.80 g, 22 mmol) are added to a solution of 1,2-bis(4-methoxyphenyl)-ethane-1,2-dione (5.4 g, 20 mmol) prepared according to example 1 in acetic acid (25 ml). The mixture is heated at reflux for 12 hours. After returning to ambient temperature, the reaction mixture is poured into water. The raw reaction product is collected by filtration and washed with water. The residue is recrystallized in acetic acid. After filtration and washing in water, 5.9 g (95%) of a yellow solid is obtained after drying. δH (200 MHz, CDCl3), 3.86 (s; 6H), 6.94 (m; 4H), 7.67 (s; 4H).

1. customprepared
2. temperatureThe mixture is heated
3. temperatureat reflux for 12 hours
4. customAfter returning to ambient temperature
5. customThe raw reaction product
6. filtrationis collected by filtration
7. washwashed with water
8. customThe residue is recrystallized in acetic acid
9. filtrationAfter filtration
10. washwashing in water