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Methanol → HCID 11380534, 화합물

HRID 2049142
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HRID 2049142 반응식
[CH2:1]([C:15](=[CH2:19])[C:16]([OH:18])=[O:17])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].B(F)(F)F.[CH3:24]O>>[CH2:1]([C:15](=[CH2:19])[C:16]([O:18][CH3:24])=[O:17])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887Methanol2회HCID 6356Boron trifluorideHCID 12731441HCID 12731441, 화합물

생성물 1

HCID 11380534HCID 11380534, 화합물

실험 절차

14.6 Grams of 2-tetradecylacrylic acid (0.052 mole) are combined with 65 ml of absolute methanol and 15 ml of 51% BF3 in methanol in a 200 ml flask equipped with a condenser and drying tube. The system is heated under reflux for six hours (two layers appear when cooled). The mixture is concentrated to 1/2 volume and the acid is neutralized with saturated NaHCO3 solution to about pH 7. The oily material is extracted with ether, washed with water and dried over anhydrous MgSO4. The ether solvent is removed under reduced pressure. The oily residue of methyl 2-tetradecylacrylate (14.70 g) is not purified further (>95% pure by GC) and used directly in the next step.

후처리

  • customequipped with a condenser
  • customdrying tube
  • temperatureThe system is heated
  • temperatureunder reflux for six hours
  • temperature(two layers appear when cooled)
  • concentrationThe mixture is concentrated to 1/2 volume
  • extractionThe oily material is extracted with ether
  • washwashed with water
  • dry with materialdried over anhydrous MgSO4
  • customThe ether solvent is removed under reduced pressure
  • customThe oily residue of methyl 2-tetradecylacrylate (14.70 g) is not purified further (>95% pure by GC)
  • 출처 및 근거

    ORD 기록
    ord-5da517cca00a45b781c8505a23870dc5
    출처 데이터셋
    uspto-grants-1980_04
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04196300

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