Reaktion #2336514

Reaktionsgleichung

water

14

METHYL 4,6-DIBROMO-3-HYDROXYPYRIDINE-2-CARBOXYLATE

sodium hydride

benzyl chloride

→

15

Ausbeute 90.6%

METHYL 4,6-DIBROMO-3-BENZYLOXYPYRIDINE-2-CARBOXYLATE

Ausbeute 90.6%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the addition
2. 2
   TemperaturThe mixture was then heated at 90° C. for six hours
3. 3
   Temperaturcooled
4. 4
   Extraktionextracted with ether (2×200 mL)
5. 5
   Waschenwashed with 2N NaOH (50 mL)
6. 6
   Trocknendried (MgSO4)
7. 7
   Sonstigethe solvent was evaporated

Vorschrift

To a stirred mixture of sodium hydride (0.6 g) in DMF (50 mL) was slowly added 14 (7.1 g). After the addition was complete, the mixture was stirred at room temperature for 15 minutes, then benzyl chloride (3.05 g) was added all at once. The mixture was then heated at 90° C. for six hours, cooled, poured into water (500 mL) and extracted with ether (2×200 mL). The ether extracts were combined, washed with 2N NaOH (50 mL), dried (MgSO4) and the solvent was evaporated to give 15 as a light yellow solid (8.3 g). Recrystallization from a small volume of methanol gave an analytical sample, m.p. 75-76° C.

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