Water → Benzenesulfonamide, 4-chloro-N-methoxy-3-nitro-

HRID 1356680ノート

反応式

HRID 1356680 の反応式
Cl.[O:2]([NH2:4])[CH3:3].[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([S:12](Cl)(=[O:14])=[O:13])=[CH:8][C:7]=1[N+:16]([O-:18])=[O:17].O>N1C=CC=CC=1>[Cl:5][C:6]1[CH:11]=[CH:10][C:9]([S:12]([NH:4][O:2][CH3:3])(=[O:14])=[O:13])=[CH:8][C:7]=1[N+:16]([O-:18])=[O:17]

参加物

5

反応物 3

HCID 962WaterHCID 7323Benzenesulfonyl chloride, 4-chloro-3-nitro-HCID 521874O-Methylhydroxylamine hydrochloride

生成物 1

HCID 18509259Benzenesulfonamide, 4-chloro-N-methoxy-3-nitro-収率 76%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Methoxylamine hydrochloride(0.90 g (10.8 mmol) was suspended in pyridine (3.0 ml). To this, under cooling with ice and with stirring, 4-chloro-3-nitrobenzenesulfonylchloride (2.56 g (10.8 mmol)) was added and the mixture was stirred under cooling with ice for one hour and at room temperature for 3 hours. Water (50.0 ml) was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was washed with dilute hydrochloric acid and water successively, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 2.02 g (76%) of 4-chloro-N-methoxy-3-nitrobenzenesulfonamide as pale yellow-white crystals.

後処理

  1. temperatureTo this, under cooling with ice
  2. stirringthe mixture was stirred
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with dilute hydrochloric acid and water successively
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a41d8b4830ee4341b537384905d23e2c
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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