反应 #70095
ord-bfee8a1339084b148a77c82b91b7385d
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度the mixture was heated
- 2温度under reflux
- 3其他for 12 h
- 4其他After that, toluene was removed under reduced pressure
- 5workup.DISSOLUTIONthe crude mixture was dissolved in chloroform (200 ml)
- 6萃取extracted with water (pH 5, 3×200 ml)
- 7干燥The combined organic layers were dried over sodium sulfate
- 8其他the volatiles were removed under reduced pressure
实验过程
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%).