Potassium Carbonate → HCID 86761923, Verbindung

HRID 448568

Reaktionsgleichung

[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[C:17]1[N:22]=[CH:21][N:20]=[C:19]([N:23]2[C:31]3[C:26](=[CH:27][C:28]([S:32]([CH3:35])(=[O:34])=[O:33])=[CH:29][CH:30]=3)[CH2:25][CH2:24]2)[CH:18]=1.C(=O)([O-])[O-].[K+].[K+]>CC(N(C)C)=O.C(Cl)Cl.[Cl-].[Na+].O>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([C:17]2[CH:18]=[C:19]([N:23]3[C:31]4[C:26](=[CH:27][C:28]([S:32]([CH3:35])(=[O:33])=[O:34])=[CH:29][CH:30]=4)[CH2:25][CH2:24]3)[N:20]=[CH:21][N:22]=2)[CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Komponenten

Reaktionsbedingungen

Temperatur: 90 °C

Versuchsvorschrift

A mixture of 7b (0.14 g, 2.1 eq), 6a (0.1 g, 0.3 mmol) and potassium carbonate (0.1 g, 2.2 eq) in 1 mL of DMA was heated up to 90° C. for 48 h then cooled down to room temperature and diluted with DCM (2 mL) and brine (2 mL). The layers were separated and the aqueous extracted with DCM (2×2 mL). The combined extracts were washed with brine (2×50 mL), dried over magnesium sulfate, filtered and evaporated. The residue was diluted with acetonitrile and purified on preparative HPLC to afford 7c.

Aufarbeitung

temperaturethen cooled down to room temperature
customThe layers were separated
extractionthe aqueous extracted with DCM (2×2 mL)
washThe combined extracts were washed with brine (2×50 mL)
dry with materialdried over magnesium sulfate
filtrationfiltered
customevaporated
additionThe residue was diluted with acetonitrile
custompurified on preparative HPLC

Quellen und Nachweise

ORD-Eintrag: ord-94807e5ba900447ca162d4865b48c8e6
Quelldatensatz: uspto-grants-2013_07
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08481731B2

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