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

HRID 1638687ノート

反応式

HRID 1638687 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7898677a8f9f48b091f54af6d8a2384a
出典データセット
uspto-grants-1989_11
特許番号
US04880806

反応ノート

読み込み中…