Sodium Bicarbonate → 7-Methoxynaphthalene-1-carbaldehyde

HRID 551777

反応式

HRID 551777 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 157882797-Methoxynaphthalene-1-carbaldehyde

試薬・触媒・溶媒 2

HCID 30318Osmium Tetroxide触媒HCID 21881883Oxolane--water (1/1)溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e06ce472994a4ea1acc720473797df9e
出典データセット
uspto-grants-2011_05
特許番号
US07947852B2

関連ノート

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