Water → 1-Methylsulfinyl-1-methylthio-2-(p-isobutylphenyl)ethylene

HRID 614247노트

반응식

HRID 614247 반응식
[CH2:1]([C:5]1[CH:12]=[CH:11][C:8]([CH:9]=O)=[CH:7][CH:6]=1)[CH:2]([CH3:4])[CH3:3].[CH3:13][S:14][CH2:15][S:16](=[O:18])[CH3:17].CC(C)([O-])C.[K+].O>C(O)(C)(C)C.C(Cl)Cl>[CH3:17][S:16]([C:15]([S:14][CH3:13])=[CH:9][C:8]1[CH:11]=[CH:12][C:5]([CH2:1][CH:2]([CH3:4])[CH3:3])=[CH:6][CH:7]=1)=[O:18]

참가 물질

7

반응물 4

HCID 962WaterHCID 99129Methyl (methylsulfinyl)methyl sulfideHCID 577537Benzaldehyde, 4-(2-methylpropyl)-HCID 23665647Potassium tert-butoxide

생성물 1

HCID 545626121-Methylsulfinyl-1-methylthio-2-(p-isobutylphenyl)ethylene수율 87.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6386tert-Butanol용매2회

실험 절차

p-Isobutylbenzaldehyde (486 mg) and 450 mg of formaldehyde dimethyl mercaptal S-oxide were dissolved in 1 ml of t-butanol, and 2.0 ml of a 0.608N t-butanol solution of potassium t-butoxide was added. The mixture was stirred at room temperature for 12 hours. Water (0.5 ml) and 50 ml of methylene chloride were added to the reaction mixture. The resulting mixture was dried over anhydrous sodium sulfate. The drying agent and the insoluble matter were removed by filtration, and the filtrate was concentrated under reduced pressure. The oily residue was chromatographed on a silica gel column using methylene chloride as an eluant to afford 701 mg of 1-methylsulfinyl-1-methylthio-2-(p-isobutylphenyl)ethylene in a yield of 87%. Samples for analysis were obtained by simple distillation of this product (at a bath temperature of 160° to 170° C./0.02 mmHg).

후처리

  1. dry with materialThe resulting mixture was dried over anhydrous sodium sulfate
  2. customThe drying agent and the insoluble matter were removed by filtration
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe oily residue was chromatographed on a silica gel column

출처 및 근거

ORD 기록
ord-7b4a58ef82c649e5ab1840a140114152
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144248

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