反应详情

2-propylpentanoic acid (40.16 g, 278.5 mmol) was mixed with butane-1-4-diol (114.65 g, 1272.2 mmol) and methyl-sulfonic acid (5 drops) in toluene (3500 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 chloroform (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 (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 chloroform (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