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

HRID 1428738ノート

反応式

HRID 1428738 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-943dac51f85845d9b70727e7e4d5244d
出典データセット
uspto-grants-2015_01
特許番号
US08937092B2

反応ノート

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