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

HRID 1356680노트

반응식

HRID 1356680 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a41d8b4830ee4341b537384905d23e2c
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586617B1

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