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

HRID 1909092

反応式

HRID 1909092 の反応式
[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

参加物

3

反応物 2

HCID 180AcetoneHCID 71059322HCID 71059322、化合物

生成物 1

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

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-0f7ff5355e9c4c48ba7e825ef06f81e9
出典データセット
uspto-grants-2013_12
特許番号
US08598358B2

関連ノート

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