Water → 2-chloro-N-methoxybenzenesulfonamide

HRID 1356686노트

반응식

HRID 1356686 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 185093192-chloro-N-methoxybenzenesulfonamide수율 64%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a4efb0fd2c384e50846b9f1491dd9f57
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586617B1

반응 노트

불러오는 중…