Water → 4'-Methoxymethoxy-2'-nitro-p-toluenesulfonanilide

HRID 1356644ノート

反応式

HRID 1356644 の反応式
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:11]=[CH:10][C:8]([NH2:9])=[C:7]([N+:12]([O-:14])=[O:13])[CH:6]=1.[C:15]1([CH3:25])[CH:20]=[CH:19][C:18]([S:21](Cl)(=[O:23])=[O:22])=[CH:17][CH:16]=1.O>N1C=CC=CC=1>[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:11]=[CH:10][C:8]([NH:9][S:21]([C:18]2[CH:19]=[CH:20][C:15]([CH3:25])=[CH:16][CH:17]=2)(=[O:23])=[O:22])=[C:7]([N+:12]([O-:14])=[O:13])[CH:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 185092024-(Methoxymethoxy)-2-nitroaniline

生成物 1

HCID 185092944'-Methoxymethoxy-2'-nitro-p-toluenesulfonanilide収率 69.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

4-Methoxymethoxy-2-nitroaniline (7.69 g (38.8 mmol)) was dissolved in 19.0 ml of pyridine. To this, p-toluenesulfonyl chloride (8.14 g (42.7 mmol)) was added with stirring at room temperature and the mixture was stirred at room temperature for 18 hours. Then, water (200.0 ml) was added to the reaction mixture, and the resulting mixture was extracted with chloroform. The extract was washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was then subjected to silica gel column chromatography with chloroform-ethanol (100:1) as eluent, to give 9.46 g (63%) of 4′-methoxymethoxy-2′-nitro-p-toluenesulfonanilide as a yellow oil.

後処理

  1. stirringthe mixture was stirred at room temperature for 18 hours
  2. extractionthe resulting mixture was extracted with chloroform
  3. washThe extract was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-cfb1ef98e7014bd8a0ace1985496ddb8
出典データセット
uspto-grants-2003_07
特許番号
US06586617B1

反応ノート

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