Water → 2-Chloro-4-(4,4-difluoropiperidin-1-yl)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidine

HRID 59091

Reaktionsgleichung

Reaktionsgleichung von HRID 59091
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[C:4]([CH2:9][O:10][CH2:11][C:12]([F:15])([F:14])[F:13])[N:3]=1.[F:16][C:17]1([F:23])[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C[O-].[Na+].O>C(#N)C.CO.CN(C=O)C>[Cl:1][C:2]1[N:7]=[C:6]([N:20]2[CH2:21][CH2:22][C:17]([F:23])([F:16])[CH2:18][CH2:19]2)[CH:5]=[C:4]([CH2:9][O:10][CH2:11][C:12]([F:15])([F:14])[F:13])[N:3]=1

Komponenten

8

Edukt 4

HCID 962WaterHCID 27583524,4-DifluoropiperidineHCID 10942334Sodium MethoxideHCID 1178209122,4-Dichloro-6-((2,2,2-trifluoroethoxy)methyl)pyrimidine

Produkt 1

HCID 1178211302-Chloro-4-(4,4-difluoropiperidin-1-yl)-6-((2,2,2-trifluoroethoxy)methyl)pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To an ice-cold solution of 2,4-dichloro-6-((2,2,2-trifluoroethoxy)methyl)pyrimidine (0.120 g, 0.46 mmol) in acetonitrile (2 mL) was a solution of 4,4-difluoropiperidine (0.217 g, 1.38 mmol) and sodium methoxide (30 wt % in methanol, 0.188 mL, 1.01 mmol) in MeOH (2 mL) added. The reaction was stirred at 0° C. for 2 hours. Water and DMF was added and the residue was purified by preparative HPLC to give the title compound as a dry film (0.110 g, 69%).

Aufarbeitung

  1. additionadded
  2. customthe residue was purified by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-379d10dffd7146a1a029057eb2a721b8
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09439904B2

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