反应详情

温度

100 °C

Dipropylene glycol monomethyl ether (444.6 grams; 3.0 mol), benzoic acid (373.7 grams; 3.06 mol), toluene (50 ml) and zirconium carbonate (2.0 grams) were placed into a 200 ml, 3-necked round bottom flask equipped with stirrer, thermometer, heating mantle, Dean Stark water trap, condenser and 10" Vigneux column. The reaction temperature was 180° C. at the beginning of the reaction and 217° C. after 6.5 hours with stirring. During that time, water (44 mls) was removed. The reaction was continued the next day for 2.5 hours at 224°-226° C. with the removal of water (56 mls.). The reaction mixture was washed at 95°-100° C. three times with sodium carbonate (15%) and then washed with water (400 ml). Then additional water (200 ml) was added and the product separated and dried at 125°, cooled to 100° C. and filtered. The desired product (694.6 grams) was obtained representing a yield of 91.8%. It assayed 99.5% with the following properties:

1. customequipped with stirrer
2. customThe reaction temperature was 180° C. at the beginning of the reaction and 217° C. after 6.5 hours
3. customDuring that time, water (44 mls) was removed
4. customfor 2.5 hours
5. customat 224°-226° C.
6. customwith the removal of water (56 mls.)
7. washThe reaction mixture was washed at 95°-100° C. three times with sodium carbonate (15%)
8. washwashed with water (400 ml)
9. additionThen additional water (200 ml) was added
10. customthe product separated
11. customdried at 125°
12. filtrationfiltered