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Sodium sulfate decahydrate → HCID 68092388, Verbindung

HRID 1772048
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1772048
[CH3:1][C:2]1[N:14]2[C:5]([C:6]3[O:7][CH2:8][CH2:9][N:10]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[C:11]=3[CH:12]=[CH:13]2)=[N:4][C:3]=1[C:22](OCC)=[O:23].[H-].[H-].[H-].[H-].[Li+].[Al+3].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[OH:23][CH2:22][C:3]1[N:4]=[C:5]2[N:14]([C:2]=1[CH3:1])[CH:13]=[CH:12][C:11]1[N:10]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:9][CH2:8][O:7][C:6]2=1
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Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 68089378HCID 68089378, Verbindung

Produkt 1

HCID 68092388HCID 68092388, VerbindungAusbeute 94,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 10-tert-butyl 4-ethyl 5-methyl-13-oxa-3,6,10-triazatricyclo[7.4.0.0{2,6}]trideca-1(9),2,4,7-tetraene-4,10-dicarboxylate (757 mg, 2.09 mmol) in 50 mL of THF was added LAH (2.364 g, 6.27 mmol) at 0° C. The mixture was stirred for 3 h at room temperature. To the mixture was added sodium sulfate decahydrate (257 mg) and the mixture was stirred for 15 min at room temperature. The solid was removed by filtration and the filtrate was concentrated. The residue was purified by reverse phase column chromatography (eluting with 15% acetonitrile in water, with 0.1% NH3.H2O) to give tert-butyl 4-(hydroxymethyl)-5-methyl-13-oxa-3,6,10-triazatricyclo[7.4.0.0{2,6}]trideca-1(9),2,4,7-tetraene-10-carboxylate (630 mg, 94% yield) as a white solid. ESI MS: m/z 320 [M+H]+.

Aufarbeitung

  1. stirringthe mixture was stirred for 15 min at room temperature
  2. customThe solid was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. customThe residue was purified by reverse phase column chromatography (eluting with 15% acetonitrile in water, with 0.1% NH3.H2O)

Quellen und Nachweise

ORD-Eintrag
ord-f5eded259c2b4ceeaf4505fadbee7efe
Quelldatensatz
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09249162B2

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