Cyclopropylamine → N-cyclopropyl-2-ethyl-3-(4-methyl-1-piperazinyl)-4-fluoro-6-nitroaniline

HRID 1638687노트

반응식

HRID 1638687 반응식
[CH2:1]([C:3]1[C:4](F)=[C:5]([N+:17]([O-:19])=[O:18])[CH:6]=[C:7]([F:16])[C:8]=1[N:9]1[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]1)[CH3:2].[F-].[K+].[CH:23]1([NH2:26])[CH2:25][CH2:24]1>C(OCC)(=O)C>[CH:23]1([NH:26][C:4]2[C:5]([N+:17]([O-:19])=[O:18])=[CH:6][C:7]([F:16])=[C:8]([N:9]3[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]3)[C:3]=2[CH2:1][CH3:2])[CH2:25][CH2:24]1

참가 물질

5

반응물 3

HCID 69828CyclopropylamineHCID 522689Potassium FluorideHCID 198411213-Ethyl-2,5-difluoro-4-(4-methyl-1-piperazinyl)nitrobenzene

생성물 1

HCID 19841167N-cyclopropyl-2-ethyl-3-(4-methyl-1-piperazinyl)-4-fluoro-6-nitroaniline

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To 3-ethyl-2,5-difluoro-4-(4-methyl-1-piperazinyl)nitrobenzene (1.12 g) are added potassium fluoride (0.24 g), N,N-dimethylsulfoxide (3.5 ml) and cyclopropylamine (0.4 ml), and the mixture is stirred at 80° to 85° C. for 1.5 hour. The reaction mixture is diluted with ethyl acetate, and the organic layer is washed with water and aqueous saturated sodium chloride and dried over magnesium sulfate and then concentrated under reduced pressure to give N-cyclopropyl-2-ethyl-3-(4-methyl-1-piperazinyl)-4-fluoro-6-nitroaniline (1.00 g), as viscous oil.

후처리

  1. washthe organic layer is washed with water and aqueous saturated sodium chloride
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7898677a8f9f48b091f54af6d8a2384a
출처 데이터셋
uspto-grants-1989_11
특허 번호
US04880806

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