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Hydrogen Peroxide → HCID 66722684, 화합물

HRID 1639531
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HRID 1639531 반응식
[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][C:10]=1[CH:19]=[O:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.OO.Cl([O-])=[O:24].[Na+]>C(#N)C>[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][C:10]=1[C:19]([OH:24])=[O:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 21840988HCID 21840988, 화합물HCID 23668197Sodium Chlorite

생성물 1

HCID 66722684HCID 66722684, 화합물수율 100%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 1.4 gm (5.2 mmol) of methyl 4-benzyloxy-3-formylbenzoate (prepared by benzylation of methyl 3-formyl-4-hydroxybenzoate) in 25 mL of acetonitrile is added an aqueous solution of NaH2PO4.2H2O (268 mg, 1.68 mmol in 3 mL of water) and 2.8 mL (5 equiv) of 30% hydrogen peroxide. To this mixture is added dropwise an aqueous solution of 79% sodium chlorite (830 mg, 7.25 mmol of NaClO2 in 7 mL of water). After 2 hr at room temperature at room temperature, the reaction mixture is concentrated to remove most of the acetonitrile. The residue is taken up in water and acidified with aqueous HCl. The aqueous acidic solution is extracted with ethyl acetate several times. The combined extracts are washed with brine and dried over Na2SO4. Rotoevaporation of solvent gives 1.5 gm (5.2 mmol) of methyl 4-benzyloxy-3-carboxybenzoate.

후처리

  1. concentrationthe reaction mixture is concentrated
  2. customto remove most of the acetonitrile
  3. extractionThe aqueous acidic solution is extracted with ethyl acetate several times
  4. washThe combined extracts are washed with brine
  5. dry with materialdried over Na2SO4

출처 및 근거

ORD 기록
ord-c188f3067f074d8a8e4c31212d69f37e
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08110570B2

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