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2-Dimethylaminopyridine → HCID 86663950, Verbindung

HRID 576883
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 576883
[CH2:1]([NH:8][C:9](=[O:16])[NH:10][CH2:11][CH2:12][C:13]([OH:15])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C.[CH2:39]([O:46][C:47]1[CH:52]=[CH:51][C:50]([CH2:53][C@H:54]([N:65]([CH3:67])[NH2:66])[C:55]([O:57][CH2:58][C:59]2[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=2)=[O:56])=[CH:49][CH:48]=1)[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1.CN(C1C=CC=CN=1)C>ClCCl.C(OCC)(=O)C>[CH2:39]([O:46][C:47]1[CH:52]=[CH:51][C:50]([CH2:53][C@H:54]([N:65]([CH3:67])[NH:66][C:13](=[O:15])[CH2:12][CH2:11][NH:10][C:9]([NH:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[O:16])[C:55]([O:57][CH2:58][C:59]2[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=2)=[O:56])=[CH:49][CH:48]=1)[C:40]1[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 218852-DimethylaminopyridineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 16227348N-(Benzylcarbamoyl)-beta-alanineHCID 86663947HCID 86663947, Verbindung

Produkt 1

HCID 86663950
HCID 86663950, Verbindung
Ausbeute 52,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittel2×HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 3-(3-benzylureido)propanoic acid (Compound VIII-1) 267 mg (1.20 mmol) in dichloromethane 5 ml, N-hydroxybenzotriazole 203 mg (1.50 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride 288 mg (1.50 mmol) were added and the mixture was stirred at room temperature for 0.5 hr. (S)-benzyl 3-(4-(benzyloxy)phenyl)-2-(1-methylhydrazinyl)propanoate (Compound XVIII-1) 390 mg (1.00 mmol) and a solution of dimethylaminopyridine 61 mg (0.50 mmol) in dichloromethane 1 ml were added to the reaction mixture and the mixture was stirred at room temperature for 3 hrs. The reaction mixture was diluted with ethyl acetate 50 ml and washed with saturated sodium bicarbonate solution 50 ml twice, water 50 ml twice and brine 50 ml and the organic phase was dried over magnesium sulfate and filtered. The mother solution was concentrated in vacuo and the residue was purified on silica gel column chromatography (Merck 60N spherical, neutral elution by chloroform:methanol=100:0 to 95:5) to obtain the title compound 0.31 g (52.0%).

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature for 3 hrs
  2. washwashed with saturated sodium bicarbonate solution 50 ml twice
  3. dry with materialwater 50 ml twice and brine 50 ml and the organic phase was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe mother solution was concentrated in vacuo
  6. customthe residue was purified on silica gel column chromatography (Merck 60N spherical, neutral elution by chloroform:methanol=100:0 to 95:5)

Quellen und Nachweise

ORD-Eintrag
ord-28b18e8f2c8b43518081154c8ff81df0
Quelldatensatz
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09040531B2

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