m-Chloroperbenzoic acid → HCID 20095449, 화합물

HRID 1770131노트

반응식

HRID 1770131 반응식
[C:1]([N:9]([CH3:19])[CH2:10][C:11]1[CH:16]=[CH:15][C:14]([S:17][CH3:18])=[CH:13][CH:12]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC1C=C(C=CC=1)C(OO)=[O:25]>ClCCl>[C:1]([N:9]([CH3:19])[CH2:10][C:11]1[CH:16]=[CH:15][C:14]([S:17]([CH3:18])=[O:25])=[CH:13][CH:12]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 20095459HCID 20095459, 화합물

생성물 1

HCID 20095449HCID 20095449, 화합물수율 56.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of N-benzoyl-N-methyl-N-(4-methylthiobenzyl)amine (6.8 g) in dichloromethane (120 ml) is added gradually m-chloroperoxybenzoic acid (5.5 g) with stirring at a temperature below 5° C. and the mixture is stirred at the same temperature for 15 minutes. After the reaction, the reaction mixture is washed successively with 5% aqueous potassium carbonate solution and aqueous sodium chloride solution, and subsequently dried over magnesium sulfate. After dichloromethane is distilled off from the mixture, the residue is purified by silica gel column chromatography (solvent; dichloromethane:methanol=100:0-100:5) to give N-benzoyl-N-methyl-N-(4-methylsulfinylbenzyl)amine (4.1 g).

후처리

  1. stirringthe mixture is stirred at the same temperature for 15 minutes
  2. customAfter the reaction
  3. washthe reaction mixture is washed successively with 5% aqueous potassium carbonate solution and aqueous sodium chloride solution
  4. dry with materialsubsequently dried over magnesium sulfate
  5. distillationAfter dichloromethane is distilled off from the mixture
  6. customthe residue is purified by silica gel column chromatography (solvent; dichloromethane:methanol=100:0-100:5)

출처 및 근거

ORD 기록
ord-02c8b208fa1d4e56a0c48e2b374002b2
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05385914

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