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Water → HCID 16225428、化合物

HRID 390599
ノート
印刷プレビュー

反応式

HRID 390599 の反応式
[CH2:1]([NH2:8])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[CH2:9]([O:11]/[C:12](=[CH:18]\[C:19]1[CH:20]=[N:21][C:22]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([N:31]([CH3:44])[C:32]([O:34]C3C=CC([N+]([O-])=O)=CC=3)=O)[CH:26]=2)=[CH:23][CH:24]=1)/[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH3:10].O.C(OCC)(=O)C>CN(C)C=O>[CH2:9]([O:11]/[C:12](=[CH:18]\[C:19]1[CH:20]=[N:21][C:22]([C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([N:31]([CH3:44])[C:32]([NH:8][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])=[O:34])[CH:26]=2)=[CH:23][CH:24]=1)/[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH3:10]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 81271-HeptanamineHCID 8857Ethyl AcetateHCID 86626078HCID 86626078、化合物

生成物 1

HCID 16225428HCID 16225428、化合物収率 54.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

0.16 mL (1.1 mmol) of n-heptylamine is added to a solution of 0.32 g (0.55 mmol) of ethyl (Z)-2-ethoxy-3-(6-{3-[methyl-(4-nitrophenoxycarbonyl)amino]phenyl}pyrid-3-yl)acrylate in 10 mL of dimethylformamide. The tube is sealed and rapidly placed in an oil bath preheated to 80° C. The reaction mixture is stirred at 80° C. for 1 hour 30 minutes. After cooling, the reaction is worked up by addition of 10 mL of water and extraction with ethyl acetate. The organic phases are combined, washed with saturated sodium chloride solution and then dried over magnesium sulfate. The solvents are evaporated off. The crude product obtained is purified by chromatography on a column of silica eluted with a 70/30 heptane/ethyl acetate mixture to give 0.14 g (54%) of ethyl (Z)-2-ethoxy-3-{6-[3-(3-heptyl-1-methylureido)phenyl]pyrid-3-yl}acrylate in the form of a colorless oil.

後処理

  1. customThe tube is sealed
  2. customrapidly placed in an oil bath
  3. custompreheated to 80° C
  4. temperatureAfter cooling
  5. washwashed with saturated sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. customThe solvents are evaporated off
  8. customThe crude product obtained
  9. customis purified by chromatography on a column of silica
  10. washeluted with a 70/30 heptane/ethyl acetate mixture

出典と根拠

ORDレコード
ord-81d44ad384f24607a3fc1ce91913cdcf
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08383652B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート