反应详情

温度

100 °C

A mixture of 4-chloro-2,6-dimethoxy-5-methylsulfanyl-pyrimidine (3.30 g, 15.0 mmol.) and dimethyl malonate (11.88 g, 90.0 mmol, 6.0 eq.) was added dropwise to slurry of sodium hydride (60% w/w) (3.67 g, 90.0 mmol, 6.0 eq) in DMF (80 ml) in ice bath at 0° C., then the reaction mixture was stirred at 100° C. for 10 hrs and dried, and the solvent was evaporated. The reaction mixture was partitioned between EA and 0.1 N HCl. The organic layer was washed with brine, dried over MgSO4, filtered and evaporated in vacuo. The resulting residue was purified by flash chromatography on silica gel (Hexane/EtOAc 6:1) to give a pale yellow oil product of 2.85 g (60.2%).

1. additionwas added dropwise
2. customat 0° C.
3. customdried
4. customthe solvent was evaporated
5. customThe reaction mixture was partitioned between EA and 0.1 N HCl
6. washThe organic layer was washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. customevaporated in vacuo
10. customThe resulting residue was purified by flash chromatography on silica gel (Hexane/EtOAc 6:1)
11. customto give a pale yellow oil product of 2.85 g (60.2%)