تفاعل #70091
ord-00a9ac1db27b40b09212abd489d8cc84
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةthe mixture was heated
- 2درجة الحرارةunder reflux
- 3أخرىfor 12 h
- 4أخرىAfter that, toluene was removed under reduced pressure
- 5workup.DISSOLUTIONthe crude mixture was dissolved in dichloromethane (200 ml)
- 6استخلاصextracted with water (pH 5, 3×200 ml)
- 7تجفيفThe combined organic layers were dried over sodium sulfate
- 8أخرىthe volatiles were removed under reduced pressure
الإجراء التجريبي
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%).