Triethylamine → HCID 178430797, Verbindung

HRID 630261Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 630261
Br[CH2:2][C:3]1[C:8]([Cl:9])=[CH:7][N:6]=[CH:5][C:4]=1[Cl:10].[CH3:11][C:12]1[C:13]([OH:19])=[N:14][C:15]([SH:18])=[N:16][CH:17]=1.C(N(CC)CC)C>C(O)C>[Cl:10][C:4]1[CH:5]=[N:6][CH:7]=[C:8]([Cl:9])[C:3]=1[CH2:2][S:18][C:15]1[N:14]=[C:13]([OH:19])[C:12]([CH3:11])=[CH:17][N:16]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 222277664-(Bromomethyl)-3,5-dichloropyridineHCID 178430804HCID 178430804, Verbindung

Produkt 1

HCID 178430797HCID 178430797, VerbindungAusbeute 100,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

To a mixture of 4-(bromomethyl)-3,5-dichloropyridine (1.0 g, 4.15 mmol) and 5-methyl-2-sulfanylpyrimidin-4-ol (0.38 g, 2.69 mmol) in anhydrous ethanol (25 mL) at 0° C. was added triethylamine (1.67 g, 16.6 mmol). The reaction mixture was stirred at room temperature overnight. The solvent was evaporated, water was added, and the mixture was sonicated and then filtered. The solid was washed with water and hexane to provide 2-{[(3,5-dichloropyridin-4-yl)methyl]sulfanyl}-5-methylpyrimidin-4-ol (0.817 g, 65% yield); 1H NMR (400 MHz, DMSO-d6): δ 1.90 (s, 3H), 4.66 (s, 2H), 7.99 (s 1H), 8.66 (s, 2H); M+302.5.

Aufarbeitung

  1. customThe solvent was evaporated
  2. additionwater was added
  3. customthe mixture was sonicated
  4. filtrationfiltered
  5. washThe solid was washed with water and hexane

Quellen und Nachweise

ORD-Eintrag
ord-92cd2a470f314cbcb03af74f4afe0c25
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09315521B2

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