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1,2-Dichloroethane → 1-benzyl-4-(benzyloxy)-N-{4-fluoro-2-[(methylamino)carbonyl]benzyl}-2-oxo-1,2-dihydro-1,5-naphthyridine-3-carboxamide

HRID 1179327
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Reaktionsgleichung

Reaktionsgleichung von HRID 1179327
[CH2:1]([N:8]1[C:17]2[C:12](=[N:13][CH:14]=[CH:15][CH:16]=2)[C:11]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[C:10]([C:26]([OH:28])=O)[C:9]1=[O:29])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1C=NC2N(O)N=NC=2C=1.C(Cl)CCl.[Cl-].[F:45][C:46]1[CH:51]=[CH:50][C:49]([CH2:52][NH3+:53])=[C:48]([C:54]([NH:56][CH3:57])=[O:55])[CH:47]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[CH2:1]([N:8]1[C:17]2[C:12](=[N:13][CH:14]=[CH:15][CH:16]=2)[C:11]([O:18][CH2:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)=[C:10]([C:26]([NH:53][CH2:52][C:49]2[CH:50]=[CH:51][C:46]([F:45])=[CH:47][C:48]=2[C:54]([NH:56][CH3:57])=[O:55])=[O:28])[C:9]1=[O:29])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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Komponenten

7

Edukt 5

HCID 111,2-Dichloroethane2×HCID 81531DiisopropylethylamineHCID 181649HOAtHCID 589780031-Benzyl-4-(benzyloxy)-2-oxo-1,2-dihydro-1,5-naphthyridine-3-carboxylic acidHCID 866001764-Fluoro-2-[(methylamino)carbonyl]benzylamine hydrochloride

Produkt 1

HCID 58977997
1-benzyl-4-(benzyloxy)-N-{4-fluoro-2-[(methylamino)carbonyl]benzyl}-2-oxo-1,2-dihydro-1,5-naphthyridine-3-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 1-benzyl-4-(benzyloxy)-2-oxo-1,2-dihydro-1,5-naphthyridine-3-carboxylic acid (0.15 g, 0.39 mmol) in DMF (4 mL) was added HOAT (0.26 g, 1.94 mmol) and EDC (0.07 g, 0.47 mmol). The solution was stirred for 10 minutes at which time EDC (0.036 g, 0.23 mmol), {4-fluoro-2-[(methylamino)carbonyl]phenyl}methanaminium chloride (0.108 g, 0.47 mmol), and DIEA (0.10 g, 0.78 mmol) were added. The reaction was then stirred at room temperature overnight at which time the solution was purified by preparative reverse phase HPLC eluting with a gradient of 5-95% acetonitrile/water (0.1% TFA). The fractions that contained the desired product were concentrated. Note that during the prep des-O-benzyl product was also obtained. The mixture was taken on to the next step.

Aufarbeitung

  1. additionwere added
  2. customwas purified by preparative reverse phase HPLC
  3. washeluting with a gradient of 5-95% acetonitrile/water (0.1% TFA)
  4. concentrationwere concentrated
  5. customwas also obtained

Quellen und Nachweise

ORD-Eintrag
ord-851879903ded4fe497ddd7f4017124e8
Quelldatensatz
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07279487B2

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