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4-Methylmorpholine → N-{4-[(2-methylpropyl)amino]quinolin-3-yl}-3-(2-methyl-1,3-dioxolan-2-yl)propanamide

HRID 599452
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 599452
[CH3:1][CH:2]([CH3:16])[CH2:3][NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=[CH:7][C:6]=1[NH2:15].[CH3:17][C:18]1([CH2:23][CH2:24][C:25](O)=[O:26])[O:22][CH2:21][CH2:20][O:19]1.CN1CCOCC1.Cl.CN(C)CCCN=C=NCC.C(=O)(O)[O-].[Na+]>CN(C=O)C.CN(C)C1C=CN=CC=1>[CH3:1][CH:2]([CH3:16])[CH2:3][NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:8]=[CH:7][C:6]=1[NH:15][C:25](=[O:26])[CH2:24][CH2:23][C:18]1([CH3:17])[O:22][CH2:21][CH2:20][O:19]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 79724-MethylmorpholineHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 109317243-(2-methyl-1,3-dioxolan-2-yl)propanoic AcidHCID 11298872N4-(2-methylpropyl)quinoline-3,4-diamine

Produkt 1

HCID 67052427
N-{4-[(2-methylpropyl)amino]quinolin-3-yl}-3-(2-methyl-1,3-dioxolan-2-yl)propanamide
Ausbeute 71,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a cooled solution of N4-(2-methylpropyl)quinoline-3,4-diamine (2.15 g, 10 mmol) in DMF (40 mL) was added 3-(2-methyl-1,3-dioxolan-2-yl)propanoic acid (2.40 g, 15 mmol), followed by 4-methylmorpholine (1.6 mL, 15 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI) (2.9 g, 15 mmol). The resulting suspension was stirred at room temperature and 4-dimethylaminopyridine (0.12 g, 1 mmol) was added. The dark yellow solution was stirred at room temperature for 16 hours, then saturated aqueous sodium bicarbonate (100 mL) was added. The mixture was transferred to a separatory funnel and was extracted with dichloromethane (2×100 mL). The organic layers were combined, washed with saturated aqueous sodium bicarbonate (100 mL) and brine (100 mL), dried over sodium sulfate, filtered, and concentrated under reduced pressure to afford an oil that was purified by flash chromatography (silica gel, elution with 5% methanol in dichloromethane) to provide 2.55 g of N-{4-[(2-methylpropyl)amino]quinolin-3-yl}-3-(2-methyl-1,3-dioxolan-2-yl)propanamide.

Aufarbeitung

  1. stirringThe dark yellow solution was stirred at room temperature for 16 hours
  2. customThe mixture was transferred to a separatory funnel
  3. extractionwas extracted with dichloromethane (2×100 mL)
  4. washwashed with saturated aqueous sodium bicarbonate (100 mL) and brine (100 mL)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customto afford an oil that
  9. customwas purified by flash chromatography (silica gel, elution with 5% methanol in dichloromethane)

Quellen und Nachweise

ORD-Eintrag
ord-e9a278939dcc4c329f7db3e1e0e77d92
Quelldatensatz
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07897767B2

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