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Acetyl chloride → HCID 21320009、化合物

HRID 262154
ノート
印刷プレビュー

反応式

HRID 262154 の反応式
[C:1](Cl)(=[O:3])[CH3:2].[N:5]1([CH:10]([O:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:11]([OH:16])[C:12]([CH3:15])([CH3:14])[CH3:13])[CH:9]=[CH:8][N:7]=[CH:6]1>C(OCC)(=O)C>[C:1]([O:16][CH:11]([C:12]([CH3:15])([CH3:14])[CH3:13])[CH:10]([O:17][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[N:5]1[CH:9]=[CH:8][N:7]=[CH:6]1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 12766922HCID 12766922、化合物

生成物 1

HCID 21320009HCID 21320009、化合物収率 68.1%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

8.0 g (0.1 mol) of acetyl chloride are added to 20.6 g (0.1 mol) of 1-imidazol-1-yl-1-phenoxy-3,3-dimethyl-butan-2-ol in 100 ml of ethyl acetate at room temperature. The mixture is then heated under reflux for 4 hours. It is allowed to cool and concentrated by distilling off the solvent in vacuo. The residue is taken up in benzene and the solution is washed with aqueous sodium bicarbonate solution and dried over sodium sulphate. The solvent is distilled off under a water pump vacuum and the residue is recrystallized from petroleum ether. 20.6 g (45% of theory) of 2-acetoxy-1-phenoxy-1-imidazol-1-yl-3,3-dimethyl-butane are obtained as a mixture of isomers with a melting point of 114°-121° C.

後処理

  1. temperatureThe mixture is then heated
  2. temperatureunder reflux for 4 hours
  3. temperatureto cool
  4. concentrationconcentrated
  5. distillationby distilling off the solvent in vacuo
  6. washthe solution is washed with aqueous sodium bicarbonate solution
  7. dry with materialdried over sodium sulphate
  8. distillationThe solvent is distilled off under a water pump vacuum
  9. customthe residue is recrystallized from petroleum ether

出典と根拠

ORDレコード
ord-357cf40c989b44bb97d86753ec770f6c
出典データセット
uspto-grants-1979_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04153708

反応ノート

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