反应详情

温度

85 °C

Dissolve 5′-chloro-2′-hydroxyacetophenone (15.3594 g, 90.03 mmol) in 100 mL of anhydrous acetonitrile in a pressure vessel. Add K2CO3 (13.7541 g, 99.52 mmol) and MeI (25.56 mL, 180.06 mmol) to the vessel. Seal the vessel and heat the reaction mixture to 85° C. for 18 hours. Cool the reaction and concentrate it in vacuo. Partition the residue between Et2O and H2O. Wash the organic layers with 2N NaOH (2×). Dry the combined organic layers with MgSO4. Filter off the drying agent and concentrate in vacuo to afford 13.15 g of 1-(5-chloro-2-methoxy-phenyl)-ethanone (79%).

1. customSeal the vessel
2. temperatureCool
3. customthe reaction
4. concentrationconcentrate it in vacuo
5. customPartition the residue between Et2O and H2O
6. washWash the organic layers with 2N NaOH (2×)
7. dry with materialDry the combined organic layers with MgSO4
8. filtrationFilter off the drying agent
9. concentrationconcentrate in vacuo