Reaktion #163375

Reaktionsgleichung

N-[2-(4-ethynyl-phenyl)-1-methyl-ethyl]-acetamide

4-iodo-2-(methylthio)pyrimidine

→

N-{1-Methyl-2-[4-(2-methylsulfanyl-pyrimidin-4-ylethynyl)-phenyl]-ethyl}acetamide

Lösungsmittel

sec-butylamine

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionextracted with DCM
2. 2
   TrocknenThe organic layer is dried with Na2SO4
3. 3
   Sonstigethe solvent is removed in vacuo
4. 4
   SonstigeThe residue is purified by column chromatography (silica gel, DCM/MeOH 96/4)
5. 5
   SonstigeThe resulting product is triturated with diethylether

Vorschrift

To 0.52 g (2.58 mmol) N-[2-(4-ethynyl-phenyl)-1-methyl-ethyl]-acetamide (I58.3) and 0.50 g (1.98 mmol) 4-iodo-2-(methylthio)pyrimidine in 3 mL sec-butylamine and 3 mL water are added 0.14 g (0.20 mmol) bis(triphenylphosphine)dichloro-palladium and the mixture is stirred at r.t. over night. The reaction mixture is diluted with water and extracted with DCM. The organic layer is dried with Na2SO4 and the solvent is removed in vacuo. The residue is purified by column chromatography (silica gel, DCM/MeOH 96/4). The resulting product is triturated with diethylether.

Quelle