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Potassium Carbonate → HCID 54080301, 화합물

HRID 1352878
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HRID 1352878 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 79177tert-Butyl bromoacetateHCID 152273Phenol, 3-(2-hydroxyethoxy)-

생성물 1

HCID 54080301HCID 54080301, 화합물수율 246%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-7f5a3a90157046ac82155f5dff90f0eb
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07220773B2

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