반응 #70091

반응 방정식

2-propylpentanoic acid

propane-1-3-diol

→

oil

수율 99.0%

3-hydroxypropyl 2-propylpentanoate

수율 99.0%

용매

toluene

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도under reflux
3. 3
   기타for 12 h
4. 4
   기타After that, toluene was removed under reduced pressure
5. 5
   workup.DISSOLUTIONthe crude mixture was dissolved in dichloromethane (200 ml)
6. 6
   추출extracted with water (pH 5, 3×200 ml)
7. 7
   건조The combined organic layers were dried over sodium sulfate
8. 8
   기타the volatiles were removed under reduced pressure

실험 절차

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%).

출처