Water → 4-acetyl-N-methoxybenzenesulfonamide

HRID 347346

반응식

HRID 347346 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][CH:5]=1)(=[O:3])[CH3:2].CCN(CC)CC.Cl.[CH3:22][O:23][NH2:24].O>C1COCC1>[C:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([NH:24][O:23][CH3:22])(=[O:12])=[O:11])=[CH:6][CH:5]=1)(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 2664184-Acetylbenzenesulfonyl chlorideHCID 521874O-Methylhydroxylamine hydrochloride

생성물 1

HCID 210825254-acetyl-N-methoxybenzenesulfonamide수율 65.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Ex-30A: To a solution of 4-acetylbenzenesulfonyl chloride (2.18 g, 10.0 mmol) in 100 ml of THF at 0° C., Et3N (2.5 g, 25 mmol) was added followed by O-methyl hydroxyamine hydrochloride (0.84 g, 10 mmol). The mixture was stirred for 1 hr at room temperature and then poured into water, and the precipitate was filtered and dried. Recrystallization from THF/hexanes gave 1.5 g (65.8%) of 4-acetyl-N-methoxybenzenesulfonamide as a white solid. 1H-NMR (300 MHz, CDCl3) δ 8.10 (d, J=8 Hz, 2H), 8.03 (d, J=8 Hz, 2H), 7.23 (brs, 1H), 3.82 (s, 3H), 2.66 (s, 3H).

후처리

  1. filtrationthe precipitate was filtered
  2. customdried
  3. customRecrystallization from THF/hexanes

출처 및 근거

ORD 기록
ord-2bd081d3498142daa8aac276c99843da
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07173129B2

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