تفاعل #70091

ord-00a9ac1db27b40b09212abd489d8cc84

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was heated
  2. 2
    درجة الحرارةunder reflux
  3. 3
    أخرىfor 12 h
  4. 4
    أخرىAfter that, toluene was removed under reduced pressure
  5. 5
    workup.DISSOLUTIONthe crude mixture was dissolved in dichloromethane (200 ml)
  6. 6
    استخلاصextracted with water (pH 5, 3×200 ml)
  7. 7
    تجفيفThe combined organic layers were dried over sodium sulfate
  8. 8
    أخرىthe 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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08535655B2uspto-grants-2013_09