Butyl bromide → N-butyl-N-acetyl-2,4-difluoroaniline

HRID 1494446

反応式

HRID 1494446 の反応式
[CH2:1](Br)[CH2:2][CH2:3][CH3:4].[OH-].[K+].[C:8]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=1[F:19])(=[O:10])[CH3:9]>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.O.C1(C)C=CC=CC=1>[CH2:1]([N:11]([C:8](=[O:10])[CH3:9])[C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:13]=1[F:19])[CH2:2][CH2:3][CH3:4]

参加物

7

反応物 3

HCID 8002Butyl bromideHCID 14797Potassium HydroxideHCID 96093Acetamide, N-(2,4-difluorophenyl)-

生成物 1

HCID 19827549N-butyl-N-acetyl-2,4-difluoroaniline収率 68.7%

試薬・触媒・溶媒 3

HCID 66133Benzyl triethylammonium chloride触媒HCID 962Water溶媒2 回HCID 1140Toluene溶媒

実験手順

0.9 g of triethylbenzylammonium chloride, 6.9 g of butyl bromide and a solution of 5.7 g of KOH in 6 ml of water are added to a stirred solution of 3.4 g of N-acetyl-2,4-difluoroaniline (Example 2) in 60 ml of toluene. The emulsion produced is warmed at 97° (reflux). After 1 h, the emulsion is cooled to room temperature and diluted with 20 ml of water. The two phases are separated, and the organic phase is dried over MgSO4 and evaporated in vacuo. The liquid crude product is purified by medium-pressure chromatography. 3.1 g of N-butyl-N-acetyl-2,4-difluoroaniline are obtained as a brownish oil.

後処理

  1. customThe emulsion produced
  2. temperatureis warmed at 97°
  3. temperature(reflux)
  4. customThe two phases are separated
  5. dry with materialthe organic phase is dried over MgSO4
  6. customevaporated in vacuo
  7. customThe liquid crude product is purified by medium-pressure chromatography

出典と根拠

ORDレコード
ord-97ddca6efec049b8af0e4bcb966496bc
出典データセット
uspto-grants-1991_06
特許番号
US05026625

関連ノート

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