1-Hydroxybenzotriazole → HCID 21084519, 화합물

HRID 348771

반응식

HRID 348771 반응식
[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]

참가 물질

6

반응물 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

생성물 1

HCID 21084519HCID 21084519, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fcdeb3cccc294ca7b5bb4b01e3dabb75
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176227B2

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