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

HRID 23588

反応式

HRID 23588 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-603affca2e4842b7b2bec7915cb213f2
出典データセット
uspto-grants-2005_02
特許番号
US06852713B2

関連ノート

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