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

HRID 1494446

반응식

HRID 1494446 반응식
[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]

참가 물질

7

반응물 3

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

생성물 1

HCID 19827549N-butyl-N-acetyl-2,4-difluoroaniline수율 68.7%

시약·촉매·용매 3

HCID 66133Benzyl triethylammonium chloride촉매HCID 962Water용매2회HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-97ddca6efec049b8af0e4bcb966496bc
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05026625

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