Allyl Alcohol → (3,4-Dichloro-phenoxy)-acetic acid allyl ester

HRID 23588

반응식

HRID 23588 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][C:12]=1[Cl:13])[O:5][CH2:6][C:7]([OH:9])=[O:8].[CH2:14](O)[CH:15]=[CH2:16]>>[CH2:16]([O:8][C:7](=[O:9])[CH2:6][O:5][C:4]1[CH:10]=[CH:11][C:12]([Cl:13])=[C:2]([Cl:1])[CH:3]=1)[CH:15]=[CH2:14]

참가 물질

3

반응물 2

HCID 7858Allyl AlcoholHCID 11495(3,4-Dichlorophenoxy)acetic acid

생성물 1

HCID 69732160(3,4-Dichloro-phenoxy)-acetic acid allyl ester수율 96.8%

실험 절차

To a solution of commercially available (3,4-dichloro-phenoxy)-acetic acid (2.65 g, 12.0 mmol) in allyl alcohol (12.0 cm3, 180 mmol) at ambient temperature under an atmosphere of dry nitrogen was added 4 drops concentrated sulfuric as a catalyst. The solution was stirred at ambient temperature for 20 hours and the volatile fractions removed in vacuo. The residue was dissolved in ethyl ether (50 cm3), washed with water (25 cm3), washed with saturated sodium bicarbonate (25 cm3), washed with brine (25 cm3), dried over magnesium sulfate, vacuum filtered and the filtrate volatile fractions removed in vacuo to afford the title compound as a colorless viscous oil (3.02 g, 96.8%) with positive ion ESI (M+H)+261.3.

후처리

  1. concentrationconcentrated sulfuric as a catalyst
  2. customthe volatile fractions removed in vacuo
  3. dissolutionThe residue was dissolved in ethyl ether (50 cm3)
  4. washwashed with water (25 cm3)
  5. washwashed with saturated sodium bicarbonate (25 cm3)
  6. washwashed with brine (25 cm3)
  7. dry with materialdried over magnesium sulfate, vacuum
  8. filtrationfiltered
  9. customthe filtrate volatile fractions removed in vacuo

출처 및 근거

ORD 기록
ord-603affca2e4842b7b2bec7915cb213f2
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852713B2

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