Reaktion #87408

Reaktionsgleichung

MTBE

2,4,6-Trichloro-5-methylpyrimidine

Tributyl(1-ethoxyvinyl)stannane

KF

→

title compound

2,4-dichloro-6-(1-ethoxyvinyl)-5-methylpyrimidine

Lösungsmittel

DMF

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solid was removed by filtration
2. 2
   Waschenwas washed with MTBE (60 mL)
3. 3
   WaschenThe organic phase was washed with water
4. 4
   Trocknendried over sodium sulfate
5. 5
   Sonstigeevaporated
6. 6
   SonstigeThe mixture was purified by column chromatography
7. 7
   Wascheneluting with DCM

Vorschrift

2,4,6-Trichloro-5-methylpyrimidine (2.0 g, 10.13 mmol) and bis(triphenylphosphine)palladium chloride (0.142 g, 0.20 mmol) in DMF (40 mL) was degased. Tributyl(1-ethoxyvinyl)stannane (3.59 mL, 10.64 mmol) was added. The mixture was heated at 100° C. for 1.5 h under nitrogen atmosphere. The mixture was poured into a solution of KF (6 g) in water (100 mL). MTBE (100 mL) was added mixture was for stirred 10 min. The solid was removed by filtration and was washed with MTBE (60 mL). The organic phase was washed with water, dried over sodium sulfate and evaporated. The mixture was purified by column chromatography eluting with DCM to give the title compound as a solid, 1.15 g (49%).

Quelle