Acetone → 1-(2,4-Difluorophenyl)-2-methylpropan-2-ol

HRID 1666172ノート

反応式

HRID 1666172 の反応式
[CH3:1][C:2]([CH3:4])=[O:3].[F:5][C:6]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:7]=1[CH2:8][Mg]Br.[Cl-].[NH4+]>C(OCC)C>[F:5][C:6]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:7]=1[CH2:8][C:2]([CH3:4])([OH:3])[CH3:1]

参加物

5

反応物 3

HCID 180AcetoneHCID 25517Ammonium ChlorideHCID 178505754HCID 178505754、化合物

生成物 1

HCID 220634481-(2,4-Difluorophenyl)-2-methylpropan-2-ol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

11.0 mL acetone, diluted with 50 mL diethyl ether, is added dropwise to a solution of 500 mL of 0.25 molar 2,4-difluorobenzylmagnesium bromide in diethyl ether within 20 minutes. Then the mixture is refluxed for 1.5 hours and then hydrolyzed with 10% ammonium chloride solution. The ether phase is separated off, washed with water, dried with sodium sulfate, and evaporated down. The fractional distillation of the residue yields the alcohol as a colorless liquid (boiling point: 70° C.-73° C./2 mmbar). Yield: 20.0 g (86%).

後処理

  1. temperatureThen the mixture is refluxed for 1.5 hours
  2. customThe ether phase is separated off
  3. washwashed with water
  4. dry with materialdried with sodium sulfate
  5. customevaporated down
  6. distillationThe fractional distillation of the residue

出典と根拠

ORDレコード
ord-450052fc9e5741648a7e967fee12cf96
出典データセット
uspto-grants-2011_10
特許番号
US08044046B2

反応ノート

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