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Acetyl chloride → HCID 21320009, 화합물

HRID 262154
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HRID 262154 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6367Acetyl chlorideHCID 12766922HCID 12766922, 화합물

생성물 1

HCID 21320009HCID 21320009, 화합물수율 68.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-357cf40c989b44bb97d86753ec770f6c
출처 데이터셋
uspto-grants-1979_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04153708

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