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Sodium Bicarbonate → 2-Hydroxymethyl-2,4,6,7-tetramethyldihydrobenzofuran

HRID 1987773
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HRID 1987773 반응식
[CH3:1][C:2](=[CH2:14])[CH2:3][C:4]1[C:9]([CH3:10])=[CH:8][C:7]([CH3:11])=[C:6]([CH3:12])[C:5]=1[OH:13].C(=O)([O-])[OH:16].[Na+]>C(Cl)Cl>[OH:16][CH2:14][C:2]1([CH3:1])[CH2:3][CH:4]2[CH:9]([CH3:10])[CH:8]=[C:7]([CH3:11])[C:6]([CH3:12])=[C:5]2[O:13]1
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참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 10655310Phenol, 2,3,5-trimethyl-6-(2-methyl-2-propenyl)-

생성물 1

HCID 688473332-Hydroxymethyl-2,4,6,7-tetramethyldihydrobenzofuran

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

31.86 g of 2-(2-methyl-2-propenyl)-3,5,6-trimethylphenol was dissolved in 600 ml of methylene chloride and 47.5 g of methchloroperbenzoic acid was gradually charged while maintaining at 0° C. After stirring at 0° C. for 2 hours, the solution was poured into an aqueous sodium hydrogen carbonate. The organic layer was extracted with chloroform, washed with an aqueous saturated sodium hydrogen carbonate solution and dried over anhydrous magnesium sulfate and, after the solvent was distilled off, the residue was purified by silica gel column chromatography (chloroform) to obtain 17 g of the objective product.

후처리

  1. extractionThe organic layer was extracted with chloroform
  2. washwashed with an aqueous saturated sodium hydrogen carbonate solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationafter the solvent was distilled off
  5. customthe residue was purified by silica gel column chromatography (chloroform)

출처 및 근거

ORD 기록
ord-2f833f6ed1534ae9b596ad94690411f9
출처 데이터셋
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07553837B2

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