Sodium Bicarbonate → 7-Methoxynaphthalene-1-carbaldehyde

HRID 551777

반응식

HRID 551777 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[CH:8][CH:9]=[C:10]2[CH:13]=C)=[CH:5][CH:4]=1.I([O-])(=O)(=O)=[O:16].[Na+].C(=O)([O-])O.[Na+]>O1CCCC1.O.[Os](=O)(=O)(=O)=O>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[CH:8][CH:9]=[C:10]2[CH:13]=[O:16])=[CH:5][CH:4]=1

참가 물질

6

반응물 3

HCID 516892Sodium BicarbonateHCID 23667635Sodium periodateHCID 445416687-Methoxy-1-vinylnaphthalene

생성물 1

HCID 157882797-Methoxynaphthalene-1-carbaldehyde

시약·촉매·용매 2

HCID 30318Osmium Tetroxide촉매HCID 21881883Oxolane--water (1/1)용매

실험 절차

The compound obtained in Step B (13.4 mmol) and osmium tetroxide (0.16 mmol) are dissolved in 70 ml of a mixture of tetrahydrofuran/water (1/1). Sodium periodate (26.9 mmol) is added in small portions and the reaction mixture is stirred for 2 hours at ambient temperature. The reaction mixture is poured into 50 ml of 5% sodium hydrogen carbonate solution, the insoluble material is filtered off and the aqueous phase is extracted twice with 75 ml of ether. The organic phase is washed with water, decolourised and evaporated. The precipitate obtained is recrystallised from cyclohexane and yields the title product in the form of a white solid.

후처리

  1. filtrationthe insoluble material is filtered off
  2. extractionthe aqueous phase is extracted twice with 75 ml of ether
  3. washThe organic phase is washed with water
  4. customevaporated
  5. customThe precipitate obtained
  6. customis recrystallised from cyclohexane

출처 및 근거

ORD 기록
ord-e06ce472994a4ea1acc720473797df9e
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947852B2

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