反应详情

2-propylpentanoic acid (10.0 g, 69.3 mmol) was mixed with propane-1-3-diol (42.1 g, 555.0 mmol) and methyl-sulfonic acid (5 drops) in toluene (200 ml) and the mixture was heated under reflux using a Dean Stark trap for 12 h. After that, toluene was removed under reduced pressure and the crude mixture was dissolved in dichloromethane (200 ml) and extracted with water (pH 5, 3×200 ml). The combined organic layers were dried over sodium sulfate and the volatiles were removed under reduced pressure giving a clear oil (14.0 g, 60.0 mmol, 99%).

1. temperaturethe mixture was heated
2. temperatureunder reflux
3. customfor 12 h
4. customAfter that, toluene was removed under reduced pressure
5. dissolutionthe crude mixture was dissolved in dichloromethane (200 ml)
6. extractionextracted with water (pH 5, 3×200 ml)
7. dry with materialThe combined organic layers were dried over sodium sulfate
8. customthe volatiles were removed under reduced pressure