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Diisopropylamine → HCID 178452034、化合物

HRID 2289053
ノート
印刷プレビュー

反応式

HRID 2289053 の反応式
C(N(CC)[CH:5]([CH3:7])[CH3:6])(C)C.[N+:10]([O-:13])(O)=[O:11].CC1C=C(C)[N:17]([C:21](N)=[NH:22])N=1.[NH2:24][CH2:25][CH2:26][C:27]([NH:29][C@H:30]1[CH2:34][CH2:33][N:32]([C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])[CH2:31]1)=[O:28].[CH:42](NC(C)C)(C)[CH3:43].[C:49]([O:52][CH2:53][CH3:54])(=[O:51])C>CN(C=O)C.ClCCl.O1CCCC1.CCOCC>[N+:10]([C:6]1[CH:5]=[CH:7][C:54]([CH2:53][O:52][C:49]([CH:25]([NH:24][C:21]([NH2:22])=[NH:17])[CH2:26][C:27]([NH:29][C@H:30]2[CH2:34][CH2:33][N:32]([C:35]([O:37][C:38]([CH3:41])([CH3:40])[CH3:39])=[O:36])[CH2:31]2)=[O:28])=[O:51])=[CH:43][CH:42]=1)([O-:13])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 7912DiisopropylamineHCID 8857Ethyl AcetateHCID 81531DiisopropylethylamineHCID 1981863,5-Dimethyl-1H-pyrazole-1-carboxamidine mononitrateHCID 57142019tert-butyl (3S)-3-(3-aminopropanoylamino)-1-pyrrolidinecarboxylate

生成物 1

HCID 178452034HCID 178452034、化合物

試薬・触媒・溶媒 4

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

Under ice cooling, N,N-diisopropylethylamine (961 μl) and 3,5-dimethylpyrazole-1-carboxamidine nitrate (1.11 g) were added to a solution of tert-butyl (3S)-3-(3-aminopropanoylamino)-1-pyrrolidinecarboxylate (1.42 g) in anhydrous N,N'-dimethylformamide (10 ml) and the mixture was stirred overnight at room temperature. The reaction mixture was poured into ether (150 ml) to give an oily precipitate. The precipitate was dissolved in anhydrous dichloromethane:anhydrous tetrahydrofuran=5:2 (70 ml). To the resulting solution, a solution of N-(4-nitrobenzyloxycarbonyl)oxy-5-norbornene-2,3-dicarboxyimide (4.35 g) in anhydrous dichloromethane (35 ml) was added dropwise under ice cooling, followed by the addition of N,N-diisopropylamine (1.90 ml). The resulting mixture was stirred overnight. To the reaction mixture, ethyl acetate was added. The resulting mixture was washed with water and saturated saline, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. The residue was suspended in methanol (50 ml). To the suspension, a 1N aqueous sodium hydroxide solution (6 ml) was added under ice cooling, followed by stirring overnight. The reaction mixture was concentrated by evaporation under reduced pressure and the residue was dissolved in ethyl acetate. The resulting solution was washed with water and saturated saline, dried over anhydrous magnesium sulfate and concentrated by evaporation under reduced pressure. The residue was separated by chromatography through a silica gel column (ethyl acetate, ethyl acetate-methanol), whereby 955 mg of the title target compound were obtained.

後処理

  1. customto give an oily precipitate
  2. stirringThe resulting mixture was stirred overnight
  3. washThe resulting mixture was washed with water and saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated by evaporation under reduced pressure
  6. additionTo the suspension, a 1N aqueous sodium hydroxide solution (6 ml) was added under ice cooling
  7. stirringby stirring overnight
  8. concentrationThe reaction mixture was concentrated by evaporation under reduced pressure
  9. dissolutionthe residue was dissolved in ethyl acetate
  10. washThe resulting solution was washed with water and saturated saline
  11. dry with materialdried over anhydrous magnesium sulfate
  12. concentrationconcentrated by evaporation under reduced pressure
  13. customThe residue was separated by chromatography through a silica gel column (ethyl acetate, ethyl acetate-methanol), whereby 955 mg of the title target compound
  14. customwere obtained

出典と根拠

ORDレコード
ord-d40b31db01024e15b02c780a0492d95c
出典データセット
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06090802

反応ノート

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