4-Chloro-3-methylphenol → 4-Chloro-3-methylphenyl acetate

HRID 47151

反応式

HRID 47151 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[CH3:9].[C:10](OC(=O)C)(=[O:12])[CH3:11]>S(=O)(=O)(O)O.O>[C:10]([O:8][C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([CH3:9])[CH:4]=1)(=[O:12])[CH3:11]

参加物

5

実験手順

43.0 g (0.30 mol) of 4-chloro-3-methylphenol, 34 ml (0.36 mol) of acetic anhydride and a few drops of concentrated sulfuric acid were stirred for 2 h at 60° C. in a 250 ml flask equipped with a reflux condenser. The reaction mixture was cooled to room temperature, poured into 200 ml of water and stirred for 1 h at room temperature. The mixture was then extracted with 400 ml of diethyl ether. The organic phase was dried over magnesium sulfate and the ether was distilled off. The raw product is subsequently distilled under reduced pressure (b.p. 65-68° C., 20 mbar).

後処理

  1. customequipped with a reflux condenser
  2. extractionThe mixture was then extracted with 400 ml of diethyl ether
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. distillationthe ether was distilled off
  5. distillationThe raw product is subsequently distilled under reduced pressure (b.p. 65-68° C., 20 mbar)

出典と根拠

ORDレコード
ord-2abe76b980254f9eb3d2fd29f5a44d81
出典データセット
uspto-grants-2004_03
特許番号
US06699405B2

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