m-Chloroperbenzoic acid → HCID 20095449、化合物

HRID 1614574ノート

反応式

HRID 1614574 の反応式
[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

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 20095459HCID 20095459、化合物

生成物 1

HCID 20095449HCID 20095449、化合物収率 56.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-560baf84d26240519a208ca4e119d479
出典データセット
uspto-grants-1993_03
特許番号
US05198448

反応ノート

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