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Aluminium lithium hydride → 7-(4-methoxybenzyl)-4-hydroxy-3-(hydroxymethyl)-1,7-naphthyridin-8(7H)-one

HRID 2092335
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2092335
[CH3:1][O:2][C:3]1[CH:26]=[CH:25][C:6]([CH2:7][N:8]2[C:17](=[O:18])[C:16]3[N:15]=[CH:14][C:13]([C:19](OCC)=[O:20])=[C:12]([OH:24])[C:11]=3[CH:10]=[CH:9]2)=[CH:5][CH:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][N:8]2[C:17](=[O:18])[C:16]3[N:15]=[CH:14][C:13]([CH2:19][OH:20])=[C:12]([OH:24])[C:11]=3[CH:10]=[CH:9]2)=[CH:25][CH:26]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 21226445Aluminium lithium hydrideHCID 178469681HCID 178469681, Verbindung

Produkt 1

HCID 1784907707-(4-methoxybenzyl)-4-hydroxy-3-(hydroxymethyl)-1,7-naphthyridin-8(7H)-oneAusbeute 37,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
-10 °C

Versuchsvorschrift

Ethyl 7-(4-methoxybenzyl)-4-hydroxy-8-oxo-7,8-dihydro-1,7-naphthyridine-3-carboxylate (4.00 g, 11 mmol) was suspended in anhydrous THF (60 ml) and the mixture was cooled down to −10° C. Lithium aluminum hydride 2M in THF (11 ml, 23 mmol) was added dropwise to the mixture. The cold bath was then removed and the reaction was stirred for two hours at room temperature. Sodium sulfate decahydrate (10 g) was added portionwise to the reaction. The mixture was stirred for 3 hours and then filtered. The cake collected in the filter funnel was extracted for 12 hours in a soxhlet apparatus in a 2:1 mixture of chloroform and methanol. The filtrate was directly loaded unto silica gel and purified by column chromatography on silica gel using a gradient of 0 to 10% metahnol in DCM to give 7-(4-methoxybenzyl)-4-hydroxy-3-(hydroxymethyl)-1,7-naphthyridin-8(7H)-one (1.3 g, 37% yield) as light yellow solid. MS(M+H)+ 313.

Aufarbeitung

  1. customThe cold bath was then removed
  2. additionSodium sulfate decahydrate (10 g) was added portionwise to the reaction
  3. stirringThe mixture was stirred for 3 hours
  4. filtrationfiltered
  5. customThe cake collected in the filter funnel
  6. extractionwas extracted for 12 hours in a soxhlet apparatus in a 2:1 mixture of chloroform and methanol
  7. custompurified by column chromatography on silica gel using a gradient of 0 to 10% metahnol in DCM

Quellen und Nachweise

ORD-Eintrag
ord-44ed2960b93d4527a0a2e6e7219df192
Quelldatensatz
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08440674B2

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