Acetone → 4-[(4-Bromophenoxy)methyl]-2,2,4-trimethyl-1,3-dioxolane

HRID 1909092노트

반응식

HRID 1909092 반응식
[Br:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][CH2:7][C:8]([CH3:12])([OH:11])[CH2:9][OH:10])=[CH:4][CH:3]=1.[CH3:15][C:16]([CH3:18])=O>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH2:7][C:8]2([CH3:12])[CH2:9][O:10][C:16]([CH3:18])([CH3:15])[O:11]2)=[CH:13][CH:14]=1

참가 물질

3

반응물 2

HCID 180AcetoneHCID 710593223-(4-Bromophenoxy)-2-methylpropane-1,2-diol

생성물 1

HCID 710593314-[(4-Bromophenoxy)methyl]-2,2,4-trimethyl-1,3-dioxolane수율 61%

실험 절차

3-(4-Bromophenoxy)-2-methylpropane-1,2-diol (261 mg, 1.00 mmol), acetone (10 mL), and a boron trifluoride diethyl ether complex (3 drops) were mixed. The mixture was then stirred at room temperature for 14 hours. A residue was obtained by concentrating the mixture under reduced pressure, and ethyl acetate and water were added thereto, followed by extraction. The organic layer was washed with a saline solution twice. A residue was obtained by concentrating the organic layer under reduced pressure, and the resulting residue was then subjected to chromatography refining (methylene chloride) using silica gel, obtaining 183 mg of the objective compound (yield: 61%).

후처리

  1. customA residue was obtained
  2. concentrationby concentrating the mixture under reduced pressure, and ethyl acetate and water
  3. additionwere added
  4. extractionfollowed by extraction
  5. washThe organic layer was washed with a saline solution twice
  6. customA residue was obtained
  7. concentrationby concentrating the organic layer under reduced pressure

출처 및 근거

ORD 기록
ord-0f7ff5355e9c4c48ba7e825ef06f81e9
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08598358B2

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