홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Methylamine → 4-fluoro-N-methylbenzene-1-sulfonamide

HRID 496595
노트
인쇄 미리보기

반응식

HRID 496595 반응식
CN.[CH2:3]([N:5](CC)CC)C.[F:10][C:11]1[CH:16]=[CH:15][C:14]([S:17](Cl)(=[O:19])=[O:18])=[CH:13][CH:12]=1>O1CCCC1.C(Cl)Cl>[CH3:3][NH:5][S:17]([C:14]1[CH:15]=[CH:16][C:11]([F:10])=[CH:12][CH:13]=1)(=[O:19])=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 6329MethylamineHCID 8471TriethylamineHCID 95884-Fluorobenzenesulfonyl chloride

생성물 1

HCID 24400544-fluoro-N-methylbenzene-1-sulfonamide수율 95.1%

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 8028Tetrahydrofuran용매
이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

실험 절차

A mixture of 125 ml of methylamine (0.25 molar) in tetrahydrofuran and 13.9 ml (0.10 mol) of triethylamine was chilled in an ice bath. To this chilled solution was added dropwise 19.4 g (0.10 mol) of 4-fluorobenzenesulfonyl chloride in 150 ml of CH2Cl2 was added and the mixture refluxed for 2 hours and then stirred overnight at room temperature. The mixture was with CH2Cl2, washed with H2O, 2N citric acid, brine and dried (Na2SO4). The solution was filtered through a pad of hydrous magnesium silicate and the filtrate concentrated to dryness under vacuum to give 18.0 g of white solid, mp 67-70° C.

후처리

  1. temperaturewas chilled in an ice bath
  2. additionwas added
  3. temperaturethe mixture refluxed for 2 hours
  4. washwashed with H2O, 2N citric acid, brine
  5. dry with materialdried (Na2SO4)
  6. filtrationThe solution was filtered through a pad of hydrous magnesium silicate
  7. concentrationthe filtrate concentrated to dryness under vacuum

출처 및 근거

ORD 기록
ord-76b8047aab694b01b80a5d6ed2ffd4d9
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06946473B2

반응 노트

불러오는 중…