1-Hydroxybenzotriazole → HCID 23155436、化合物

HRID 348754

反応式

HRID 348754 の反応式
[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([OH:15])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN=C=N[CH2:21][CH2:22][CH2:23][N:24]([CH3:26])C.Cl.[CH:28]1[CH:29]=[CH:30][C:31]2N(O)N=[N:34][C:32]=2C=1>C(Cl)(Cl)Cl>[CH3:1][O:5][C:6](=[O:7])[C:29]1[CH:30]=[CH:31][C:32]([NH:34][C:13](=[O:15])[CH2:12][CH2:11][CH2:10][CH2:9][NH:8][C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])=[C:26]([NH:24][CH2:23][CH2:22][CH3:21])[CH:28]=1

参加物

5

反応物 3

HCID 757711-HydroxybenzotriazoleHCID 5458485-(((Tert-butoxy)carbonyl)amino)pentanoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 23155436HCID 23155436、化合物収率 100.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

In chloroform (10 ml), 5-t-butoxycarbonylaminovaleric acid (574 mg), WSCI hydrochloride (690 mg), and HOBt (487 mg) were dissolved. Then, the resulting solution was stirred at room temperature for 30 minutes. The solution was added with 4-amino-3-propylaminobenzoic acid methyl (503 mg) and stirred overnight at room temperature. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was then dissolved in chloroform. After having been washed with a saturated aqueous sodium bicarbonate solution, a saturated aqueous ammonium chloride solution, and saturated saline solution, the solution was dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure and the residue was then purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (540 mg) as a colorless viscous substance.

後処理

  1. stirringstirred overnight at room temperature
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure
  4. dissolutionthe residue was then dissolved in chloroform
  5. washAfter having been washed with a saturated aqueous sodium bicarbonate solution
  6. dry with materiala saturated aqueous ammonium chloride solution, and saturated saline solution, the solution was dried with anhydrous sodium sulfate
  7. filtrationAfter filtration
  8. distillationthe solvent was distilled off under reduced pressure
  9. customthe residue was then purified through silica gel column chromatography (chloroform/ethyl acetate)

出典と根拠

ORDレコード
ord-7b47f229a8154903a13ddef6064e2086
出典データセット
uspto-grants-2007_02
特許番号
US07176227B2

関連ノート

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