反应详情

A mixture of 0.34 g (0.92 mMol) of 1,2-dihydro-6-(4-fluorophenyl)-5-[4-(methylthio)phenyl]-2-oxo-pyridine-3-carbonitrile (Step 3) in 10 ml of DMF and 0.33 g of K2CO3 and 2 ml of iodomethane, was stirred at room temperature over the weekend. The reaction mixture was diluted with 75 ml of water and extracted with dichloromethane (4×25 ml). The combined organic layers were extracted once with 50 ml of 10% NaOH solution then once with brine, dried over MgSO4 and evaporated to dryness. The residue was purified by HPLC to give two fractions. The first fraction was the desired product: m.p. 202.5°-204° C.

1. extractionextracted with dichloromethane (4×25 ml)
2. extractionThe combined organic layers were extracted once with 50 ml of 10% NaOH solution
3. dry with materialonce with brine, dried over MgSO4
4. customevaporated to dryness
5. customThe residue was purified by HPLC
6. customto give two fractions