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Ethyl bromoacetate → Ethyl [4-(2,2,2-trifluoro-1,1-dimethylethyl)phenoxy]acetate

HRID 1350815
ノート
印刷プレビュー

反応式

HRID 1350815 の反応式
[F:1][C:2]([F:14])([F:13])[C:3]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)([CH3:5])[CH3:4].C(=O)([O-])[O-].[K+].[K+].Br[CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24]>CN(C)C=O>[F:1][C:2]([F:13])([F:14])[C:3]([C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])=[CH:8][CH:7]=1)([CH3:5])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 220907484-(1,1,1-Trifluoro-2-methylpropan-2-yl)phenol

生成物 1

HCID 86604944Ethyl [4-(2,2,2-trifluoro-1,1-dimethylethyl)phenoxy]acetate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of 4-(2,2,2-trifluoro-1,1-dimethylethyl)phenol (408 mg, 2.0 mmol, WO 9708144A1) and potassium carbonate (552 mg, 4.0 mmol) in N,N-dimethylformamide (DMF) (30 ml) was added ethyl bromoacetate (334 mg, 2.0 mmol) and the mixture was stirred for 3 hours at ambient temperature. The reaction was partitioned with water and a 1:10 by volume mixture of ethylacetate/hexane, and the organic layer was separated and dried over sodium sulfate. After filtration to separate solvent and sodium sulfate, the solvent was removed under reduced pressure to give a residue, which was passed through a silica gel chromatography column and eluted with a 1:1 by volume mixture of ethyl acetate/hexane to furnish ethyl [4-(2,2,2-trifluoro-1,1-dimethylethyl)phenoxy]acetate. Then, ethyl [4-(2,2,2-trifluoro-1,1-dimethylethyl)phenoxy]acetate was treated with 2M aqueous sodium hydroxide (3.0 ml) and methanol (3.0 ml) for 2 hours at room temperature and was quenched with 2M aqueous hydrogen chloride to acidify the mixture adjusting to pH 1. Crude product was extracted with ethyl acetate, and then the organic layer was dried over magnesium sulfate. After filtration, solvent was evaporated under reduced pressure to give 345 mg (66% yield) of the title compound as a white solid.

後処理

  1. customThe reaction was partitioned with water
  2. additiona 1:10 by volume mixture of ethylacetate/hexane
  3. customthe organic layer was separated
  4. dry with materialdried over sodium sulfate
  5. filtrationAfter filtration
  6. customto separate solvent and sodium sulfate
  7. customthe solvent was removed under reduced pressure
  8. customto give a residue, which
  9. washeluted with a 1:1 by volume mixture of ethyl acetate/hexane

出典と根拠

ORDレコード
ord-51558433c72d47109338b181d0849f95
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07214824B2

反応ノート

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