Sodium Sulfite → HCID 13596601、化合物

HRID 260879ノート

反応式

HRID 260879 の反応式
Cl[C:2]1C=CC=C(C(OO)=O)C=1.[CH3:12][O:13][CH:14]([O:23][CH3:24])[C:15]1[CH:20]=[CH:19][C:18](SC)=[CH:17][CH:16]=1.C(=O)([O-])O.[Na+].[S:30]([O-:33])([O-])=[O:31].[Na+].[Na+]>ClCCl>[CH3:24][O:23][CH:14]([O:13][CH3:12])[C:15]1[CH:16]=[CH:17][C:18]([S:30]([CH3:2])(=[O:33])=[O:31])=[CH:19][CH:20]=1

参加物

6

反応物 4

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 135965971-(Dimethoxymethyl)-4-(methylsulfanyl)benzene

生成物 1

HCID 13596601HCID 13596601、化合物収率 93%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

m-Chloroperbenzoic acid (115.0 g, 0.567 mol) was added to a suspension of the 4-(methylthio)benzaldehyde dimethyl acetal (50.0 g, 0.252 mol) prepared in Preparative Example 1 and sodium hydrogencarbonate (73.1 g) in dichloromethane (1.00 l) at 0° to 10° C. in portions (over a period of about one hour and 20 minutes). The obtained suspension was stirred at room temperature for 18 hours and poured into an aqueous solution (1 l) of sodium sulfite (100.0 g) under cooling to decompose excess peracid. The resulting solution was extracted with dichloromethane and the organic layer was washed with a saturated aqueous solution of common salt, dried over magnesium sulfate and concentrated in a vacuum. The obtained solid residue was recrystallized from hexane/isopropyl ether/ethyl acetate to give the title compound as a colorless crystal (53.9 g, yield: 93%).

後処理

  1. custom20 minutes
  2. temperatureunder cooling
  3. extractionThe resulting solution was extracted with dichloromethane
  4. washthe organic layer was washed with a saturated aqueous solution of common salt
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in a vacuum
  7. customThe obtained solid residue was recrystallized from hexane/isopropyl ether/ethyl acetate

出典と根拠

ORDレコード
ord-500af003bf274e79a49687c600829137
出典データセット
uspto-grants-1996_06
特許番号
US05530118

反応ノート

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