反应详情

温度

20 °C

Hexadecanedioic acid (20.0 g, 69.8 mmol) and Dowex® were suspended in n-octane and heated to reflux. Benzyl formate (22.0 g, 162 mmol) was added. After 6 hours additional benzyl formate (22.0 g, 162 mmol) was added. The heating was continued for 50 hours. The reaction mixture was filtered at 80° C. The filtrate was cooled to 20° C., and the precipitate was collected by filtration. The crude product (20.2 g) was suspended in dichloromethane (220 ml) at 20° C. for 4 hours. The suspension was filtered, and the filtrate was evacuated to dryness at 20-30° C. The resulting solid (13.9 g) was recrystallised from 2-propanol (140 ml). The product was isolated by filtration, and dried to constant weight under reduced pressure at 30-40° C. Yield: 10.2 g (39%) of white material.

1. temperatureheated to reflux
2. filtrationThe reaction mixture was filtered at 80° C
3. filtrationthe precipitate was collected by filtration
4. waitThe crude product (20.2 g) was suspended in dichloromethane (220 ml) at 20° C. for 4 hours
5. filtrationThe suspension was filtered
6. customthe filtrate was evacuated to dryness at 20-30° C
7. customThe resulting solid (13.9 g) was recrystallised from 2-propanol (140 ml)
8. customThe product was isolated by filtration
9. customdried to constant weight under reduced pressure at 30-40° C