反应详情

温度

10 °C

Vanillin (2.432 kg) was added to a solution of sodium hydroxide (640 g) in water (8 l) and cooled to 10° C. with an ice-bath. Then a solution of hydrogen peroxide (30%) (2.4 1) was added at a rate to keep the temperature of the reacting mixture below 30° C. The addition completed (about 2 hours), the reaction mixture was added over a period of 3 hours to a suspension of sodium periodate (880 g) in water (4 l) and acetic acid (640 ml) cooled with an ice-bath to 10° C. (the temperature of the reacting mixture was kept below 35° C.). The resulting precipitate was filtered, washed with cold water followed by ethanol/hexane (1:1) mixture and air-dried to afford the title compound (1.9 kg), m.p. 144°-147° C.

1. customthe temperature of the reacting mixture below 30° C
2. additionThe addition
3. custom(about 2 hours)
4. temperaturecooled with an ice-bath to 10° C. (the temperature of the reacting mixture
5. customwas kept below 35° C.
6. filtrationThe resulting precipitate was filtered
7. washwashed with cold water
8. customair-dried