Methanesulfonyl chloride → N-(4-bromo-2-fluorobenzyl)methanesulfonamide

HRID 1428722ノート

反応式

HRID 1428722 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH2:9])=[C:4]([F:10])[CH:3]=1.[CH3:11][S:12](Cl)(=[O:14])=[O:13]>N1C=CC=CC=1.ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][S:12]([CH3:11])(=[O:14])=[O:13])=[C:4]([F:10])[CH:3]=1

参加物

5

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 3770848(4-Bromo-2-fluorophenyl)methanamine

生成物 1

HCID 70847718N-(4-bromo-2-fluorobenzyl)methanesulfonamide収率 94.2%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 4-bromo-2-fluorophenyl-methanamine (5.834 g, 28.592 mmol) in pyridine was added methanesulfonyl chloride (4.2 mL, 54.325 mmol) at 0° C. The reaction mixture was stirred for 1 h, then diluted with dichloromethane. The mixture was washed with water. The organic layer was dried over magnesium sulfate and filtered. The filtrate removed in vacuo. The crude was purified by column chromatography. N-(4-bromo-2-fluorobenzyl)methanesulfonamide (7.597 g) was obtained as 93% yield.

後処理

  1. washThe mixture was washed with water
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationfiltered
  4. customThe filtrate removed in vacuo
  5. customThe crude was purified by column chromatography

出典と根拠

ORDレコード
ord-6db461efc2d94a5da7a413f9b4cebbf5
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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