1-Hydroxybenzotriazole → HCID 21084519、化合物

HRID 348771

反応式

HRID 348771 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=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.[NH2:38][C:39]1[CH:40]=[C:41]([CH:44]=[CH:45][C:46]=1[NH:47][CH2:48][CH2:49][CH3:50])[C:42]#[N:43]>C(Cl)(Cl)Cl>[C:1]([O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13](=[O:15])[NH:38][C:39]1[CH:40]=[C:41]([C:42]#[N:43])[CH:44]=[CH:45][C:46]=1[NH:47][CH2:48][CH2:49][CH3:50])([CH3:2])([CH3:3])[CH3:4]

参加物

6

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 5458485-(((Tert-butoxy)carbonyl)amino)pentanoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 223802993-Amino-4-(propylamino)benzonitrile

生成物 1

HCID 21084519HCID 21084519、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

In chloroform (5.0 ml), 5-t-butoxycarbonylaminovaleric acid (387 mg), WSCI hydrochloride (466 mg), and HOBt (328.3 mg) were dissolved. Then, the solution was stirred at room temperature for 1 hour. A solution (3.0 ml) of 3-amino-4-propylaminobenzonitrile (283 mg) in chloroform was dropped in this solution. Then, the solution was stirred overnight at room temperature. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was dissolved in chloroform and then washed with a saturated aqueous sodium bicarbonate solution, a saturated aqueous ammonium chloride solution, and saturated saline solution, followed by drying 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 as a colorless viscous substance.

後処理

  1. stirringThen, the solution was stirred overnight at room temperature
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure
  4. dissolutionThe residue was dissolved in chloroform
  5. washwashed with a saturated aqueous sodium bicarbonate solution
  6. dry with materialby drying 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)
  10. customobtaining the subject compound as a colorless viscous substance

出典と根拠

ORDレコード
ord-fcdeb3cccc294ca7b5bb4b01e3dabb75
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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