Sodium Sulfite → HCID 13596601, 화합물

HRID 260879노트

반응식

HRID 260879 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 13596601HCID 13596601, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-500af003bf274e79a49687c600829137
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05530118

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