反应详情

温度

100 °C

Isodecyl alcohol (306 grams; 1.94 moles), benzoic acid (242 grams; 1.98 moles), toluene (50 ml) and butyltinoxide hydrate (1 gram) were placed into a glass reaction flask equipped with stirrer, thermometer, heating mantle, 12" column packed with 1/4" glass rings, Dean-Stark water trap and condenser. The mixture was stirred for four hours allowing the temperature to increase from 30° C. to 204° C. After reaction mixture was cooled to 100° C., soda ash (100 ml; 20% solution) was added and the temperature increased from 65° to 95° C. After ten minutes, the alkaline bottom layer was separated and a mixture of soda ash (50 ml; 20% solution) and chlorox (140 ml) added to the reaction mixture. After the bottom layer was removed, the mixture was dried and the toluene was removed by heating to 182° C. at 45 mmHg. The desired product (491 grams) was obtained after filtration representing a yield of 96.7%.

1. customequipped with stirrer
2. temperaturethermometer, heating mantle, 12" column
3. temperatureto increase from 30° C. to 204° C
4. customAfter reaction mixture
5. temperaturethe temperature increased from 65° to 95° C
6. waitAfter ten minutes
7. customthe alkaline bottom layer was separated
8. additiona mixture of soda ash (50 ml; 20% solution) and chlorox (140 ml)
9. additionadded to the reaction mixture
10. customAfter the bottom layer was removed
11. customthe mixture was dried
12. customthe toluene was removed
13. temperatureby heating to 182° C. at 45 mmHg