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

HRID 506559노트

반응식

HRID 506559 반응식
[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]

참가 물질

5

반응물 3

HCID 180AcetoneHCID 25517Ammonium ChlorideHCID 178505754HCID 178505754, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-5650b1ae737f4f768257db5092b9bd89
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786111B2

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