反応 #2345326

ord-b52d24b078eb4fa2883462d1a856be8a

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他equipped with a stirrer and a dropping funnel
  2. 2
    workup.ADDITION32.39 g (0.385 mol) of dihydropyan was dropped
  3. 3
    workup.ADDITIONAfter the completion of the addition
  4. 4
    workup.STIRRINGthe mixture was stirred at room temperature for additional 1 hour
  5. 5
    その他the reaction
  6. 6
    ろ過filtered
  7. 7
    workup.DISTILLATIONAfter distilling off the solvent

実験手順

100.26 g (0.35 mol) of methyl 16-hydroxyhexadecanoate, 0.60 g (3.5 mol) of p-toluenesulfonic acid and 350 ml of dichloromethane were introduced into a 1-1 flask equipped with a stirrer and a dropping funnel and 32.39 g (0.385 mol) of dihydropyan was dropped thereto under stirring at 0° C. After the completion of the addition, the mixture was stirred at room temperature for additional 1 hour to thereby complete the reaction. Next, the reaction mixture was neutralized by adding 0.59 g (7 mmol) of NaHCO3 and filtered. After distilling off the solvent, crude methyl 16-(2-tetrahydropyranyloxy)hexadecanoate (III-a) was obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05659052uspto-grants-1997_08