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Potassium Carbonate → HCID 54080301、化合物

HRID 1352878
ノート
印刷プレビュー

反応式

HRID 1352878 の反応式
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21]>O1CCCC1>[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:8]=[CH:9][CH:10]=1)[O:11][CH2:19][C:20]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[O:21]
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 11430Potassium CarbonateHCID 79177tert-Butyl bromoacetateHCID 152273Phenol, 3-(2-hydroxyethoxy)-

生成物 1

HCID 54080301HCID 54080301、化合物収率 246%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 3-(2-hydroxyethoxy)phenol (864 mg, 5 mmol) in tetrahydrofuran (20 ml) were added potassium carbonate (967 mg, 7 mmol) and t-butyl bromoacetate (0.89 ml, 6 mmol), and the mixture was stirred for 2 hours at room temperature. The reaction was quenched by 10% aqueous citric acid solution and the mixture was extracted with ethyl acetate. The organic layer was washed with water, 10% aqueous citric acid solution, an aqueous saturated sodium hydrogencarbonate solution and an aqueous saturated sodium chloride solution. The organic layer was dried over sodium sulfate. The solvent was removed under reduced pressure and the residue was purified with silica gel chromatography (hexane:ethyl acetate=3:1) to give the subject compound (3.30 g, 69%).

後処理

  1. customThe reaction was quenched by 10% aqueous citric acid solution
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water, 10% aqueous citric acid solution
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified with silica gel chromatography (hexane:ethyl acetate=3:1)

出典と根拠

ORDレコード
ord-7f5a3a90157046ac82155f5dff90f0eb
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07220773B2

反応ノート

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