Sodium Bicarbonate → HCID 178455311, Verbindung

HRID 1873567Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1873567
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH:10]2[CH2:15][CH2:14][CH:13]([O:16][Si:17]([C:20]([CH3:23])([CH3:22])[CH3:21])([CH3:19])[CH3:18])[CH2:12][CH2:11]2)[C:5]([C:24]#[N:25])=[C:4]([SH:26])[N:3]=1.Cl.[Cl-].C(=O)(O)[O-].[Na+]>CN(C=O)C>[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([C@H:10]2[CH2:11][CH2:12][C@@H:13]([O:16][Si:17]([C:20]([CH3:22])([CH3:23])[CH3:21])([CH3:18])[CH3:19])[CH2:14][CH2:15]2)[C:5]([C:24]#[N:25])=[C:4]([S:26][CH2:8][C:7]2[CH:2]=[N:3][CH:4]=[CH:5][CH:6]=2)[N:3]=1

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 6410751Hydrogen chloride dimerHCID 1784550312-Amino-4-(4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-6-mercaptopyridine-3,5-dicarbonitrile

Produkt 1

HCID 178455311HCID 178455311, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

97 mg (0.23 mmol) of the compound from Example 12A (cis isomer), 46 mg (0.28 mmol) of 3-pyridinemethyl chloride hydrochloride and 78 mg (0.93 mmol) of sodium bicarbonate are initially charged in 2 ml of dry DMF and stirred at RT for 20 h. The mixture is then filtered and the filtrate is directly purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5).

Aufarbeitung

  1. filtrationThe mixture is then filtered
  2. customthe filtrate is directly purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5)

Quellen und Nachweise

ORD-Eintrag
ord-d4aef8cd923d4cbea1d0936d25f682a3
Quelldatensatz
uspto-grants-2012_11
Patentnummer
US08304412B2

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