Potassium Iodide → 2-Acetonyloxy-4-chloro-3-fluoronitrobenzene

HRID 851083ノート

反応式

HRID 851083 の反応式
[Cl:1][C:2]1[C:3]([F:12])=[C:4]([OH:11])[C:5]([N+:8]([O-:10])=[O:9])=[CH:6][CH:7]=1.Cl[CH2:14][C:15](=[O:17])[CH3:16].[I-].[K+]>CC(C)=O>[CH2:14]([O:11][C:4]1[C:3]([F:12])=[C:2]([Cl:1])[CH:7]=[CH:6][C:5]=1[N+:8]([O-:10])=[O:9])[C:15]([CH3:16])=[O:17]

参加物

5

反応物 3

HCID 4875Potassium IodideHCID 6571ChloroacetoneHCID 131885853-Chloro-2-fluoro-6-nitrophenol

生成物 1

HCID 131885862-Acetonyloxy-4-chloro-3-fluoronitrobenzene収率 54.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 3 g (15.7 mmols) of 3-chloro-2-fluoro-6-nitrophenol, 3 ml of chloroacetone and 300 mg of potassium iodide in 50 ml of acetone was refluxed for 6 hours while vigorously stirring. After cooling, any insoluble substance was removed by filtration, and the filtrate was concentrated and purified by silica gel (20 g) column chromatography using chloroform as an eluant to provide 2.5 g (54.5% yield) of 2-acetonyloxy-4-chloro-3-fluoronitrobenzene as an oil.

後処理

  1. temperaturewas refluxed for 6 hours
  2. temperatureAfter cooling
  3. customany insoluble substance was removed by filtration
  4. concentrationthe filtrate was concentrated
  5. custompurified by silica gel (20 g) column chromatography

出典と根拠

ORDレコード
ord-e7ae9a4e404c437991836646a990e61b
出典データセット
uspto-grants-1983_05
特許番号
US04382892

反応ノート

読み込み中…