Water → 2-chloro-N-methoxybenzenesulfonamide

HRID 1356686

反応式

HRID 1356686 の反応式
Cl.[O:2]([NH2:4])[CH3:3].[Cl:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[S:12](Cl)(=[O:14])=[O:13].O>N1C=CC=CC=1>[Cl:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[S:12]([NH:4][O:2][CH3:3])(=[O:14])=[O:13]

参加物

5

反応物 3

HCID 962WaterHCID 761872-Chlorobenzenesulfonyl chlorideHCID 521874O-Methylhydroxylamine hydrochloride

生成物 1

HCID 185093192-chloro-N-methoxybenzenesulfonamide収率 64%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Methoxylamine hydrochloride (0.95 g (11.4 mmol)) was suspended in pyridine (4.0 ml). To this, under cooling with ice and with stirring, 2-chlorobenzenesulfonyl chloride (2.11 g (10.0 mmol)) was added and the mixture was stirred under cooling with ice for one hour and at room temperature for one hour. Water (50.0 ml) was added to the reaction mixture and the resulting mixture was extracted with ethyl acetate. The extract was washed with water, dilute hydrochloric acid and a saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 1.41 g (64%) of 2-chloro-N-methoxybenzenesulfonamide as pale yellow crystals.

後処理

  1. temperatureTo this, under cooling with ice
  2. stirringthe mixture was stirred
  3. extractionthe resulting mixture was extracted with ethyl acetate
  4. washThe extract was washed with water, dilute hydrochloric acid
  5. dry with materiala saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a4efb0fd2c384e50846b9f1491dd9f57
出典データセット
uspto-grants-2003_07
特許番号
US06586617B1

関連ノート

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