Water → 3,4-difluoro-N-methylbenzene-1-sulfonamide

HRID 1964593노트

반응식

HRID 1964593 반응식
[F:1][C:2]1[CH:3]=[C:4]([S:9](Cl)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8].Cl.CN.[CH2:16]([N:18](CC)CC)C.O>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([S:9]([NH:18][CH3:16])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 27369133,4-Difluorobenzene-1-sulfonyl chlorideHCID 6364545Methylamine hydrochloride

생성물 1

HCID 84679853,4-difluoro-N-methylbenzene-1-sulfonamide수율 30%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Commercially available 3,4-difluorophenylsulfonylchloride (117 μL, 0.87 mmol) was dissolved in dichloromethane (5 mL), and methylamine hydrochloride (49 mg, 0.73 mmol) and triethylamine (203 μL, 1.45 mmol) were added, followed by stirring at room temperature for 2 hours. To the reaction solution, water (15 mL) was added, extraction was carried out twice with dichloromethane (15 mL), and washing was carried out with saturated brine (15 mL), followed by drying over sodium sulfate. The solvent was distilled off under reduced pressure, followed by vacuum drying, to afford the desired compound (44.7 mg, yield 30%) as a colorless oil.

후처리

  1. extractionextraction
  2. washwashing
  3. dry with materialby drying over sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customdrying

출처 및 근거

ORD 기록
ord-82d86fa2c9cc4f4897aab3ac305771ba
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415359B2

반응 노트

불러오는 중…