反应详情

温度

22.5 °C

2,2-bis(hydroxymethyl)propionic acid (10 g) and anisaldehyde dimethyl acetal (20.4 g) were added to acetone (50 ml) at 20-25° C. p-Toluenesulfonic acid (0.51 g) was added to the reaction mixture and stirred at 20-25° C. for 5 hours. The mixture was then cooled to 0-5° C. and stirred for 1 hour. The slurry was filtered and the solid was washed with chilled (0-5° C.) acetone (10 ml). The solid was dried under vacuum at 45-50° C. for 4 hour. The solid was added to toluene (150 ml) and the resulting mixture was heated at 65-70° C. for 2 hours. The mixture was then cooled to 5-10° C. and stirred for 30 minutes. The slurry was filtered and the solid was washed with toluene (10 ml) followed by drying under vacuum at 30-35° C. for 4 hours to obtain title compound (14.0 g, 74.4%).

1. additionwas added to the reaction mixture
2. temperatureThe mixture was then cooled to 0-5° C.
3. stirringstirred for 1 hour
4. filtrationThe slurry was filtered
5. washthe solid was washed
6. temperaturewith chilled (0-5° C.) acetone (10 ml)
7. customThe solid was dried under vacuum at 45-50° C. for 4 hour
8. additionThe solid was added to toluene (150 ml)
9. temperaturethe resulting mixture was heated at 65-70° C. for 2 hours
10. temperatureThe mixture was then cooled to 5-10° C.
11. stirringstirred for 30 minutes
12. filtrationThe slurry was filtered
13. washthe solid was washed with toluene (10 ml)
14. customby drying under vacuum at 30-35° C. for 4 hours