Methanesulfonyl chloride → N-(2-fluoro-4-nitrobenzyl)methanesulfonamide

HRID 1428738노트

반응식

HRID 1428738 반응식
[F:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[CH2:11][NH2:12].[CH3:13][S:14](Cl)(=[O:16])=[O:15]>N1C=CC=CC=1.ClCCl>[F:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[CH2:11][NH:12][S:14]([CH3:13])(=[O:16])=[O:15]

참가 물질

5

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 45121148(2-Fluoro-4-nitrophenyl)methanamine

생성물 1

HCID 86679366N-(2-fluoro-4-nitrobenzyl)methanesulfonamide수율 88.3%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매

실험 절차

To a stirred solution of (2-fluoro-4-nitrophenyl)methanamine (194 mg, 1.140 mmol) in pyridine, cooled to 0° C., were added methanesulfonyl chloride (248 mg, 2.166 mmol). The resulting reaction mixture was stirred for 1 h at room temperature. The mixture was dissolved in dichloromethane and washed with 1N HCl. The organic layer was dried over magnesium sulfate and filtered. The filtrate removed in vacuo. The crude was purified by column chromatography. N-(2-Fluoro-4-nitrobenzyl)methanesulfonamide (250 mg) was obtained as 88% yield.

후처리

  1. customThe resulting reaction mixture
  2. washwashed with 1N HCl
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. customThe filtrate removed in vacuo
  6. customThe crude was purified by column chromatography

출처 및 근거

ORD 기록
ord-943dac51f85845d9b70727e7e4d5244d
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937092B2

반응 노트

불러오는 중…