Hydrochloric Acid → N-(2-Fluoro-4-iodophenyl)methanesulfonamide

HRID 656266

反応式

HRID 656266 の反応式
[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH2:9].N1C=CC=CC=1.[CH3:16][S:17](Cl)(=[O:19])=[O:18].Cl>ClCCl>[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH:9][S:17]([CH3:16])(=[O:19])=[O:18]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 1856942-Fluoro-4-iodoaniline

生成物 1

HCID 19785608N-(2-Fluoro-4-iodophenyl)methanesulfonamide収率 95%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-fluoro-4-iodophenylamine (1.50 g) was dissolved in dichloromethane (40 ml) and to the solution were added pyridine (1.02 ml) and methanesulfonylchloride (700 μl). The mixture was stirred at room temperature for 1 hour and 1.5 N aqueous hydrochloric acid was added thereto to quench the reaction. The resulting mixture was extracted with dichloromethane, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The obtained residue was column-chromatographed (ethyl acetate/hexane=1/1) to yield the compound 3-2 (1.89 g, 95%).

後処理

  1. customto quench
  2. customthe reaction
  3. extractionThe resulting mixture was extracted with dichloromethane
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe obtained residue was column-chromatographed (ethyl acetate/hexane=1/1)

出典と根拠

ORDレコード
ord-e456631fb3dd416e8419fec0356e2fa2
出典データセット
uspto-grants-2011_12
特許番号
US08071650B2

関連ノート

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