反应详情

To a solution of diethyl malonate (1.67 g, 10.4 mmol) in EtOH (30 mL) at r.t. was added sodium methoxide (2.26 mL, 25% solution in MeOH). The mixture was stirred for 5 minutes and a solution of the compound of Step 3 (1.3 g, 4.2 mmol) in EtOH (10 mL) was added. The mixture was stirred at 75° C. for 12 hours, saturated aqueous NH4Cl was added and the aqueous layer was extracted with EtOAc. The combined organic layers were dried over Na2SO4 and concentrated. The residue was purified by silica gel chromatography eluted with 20% EtOAc to give 1.6 g of the title compound.

1. stirringThe mixture was stirred at 75° C. for 12 hours
2. extractionthe aqueous layer was extracted with EtOAc
3. dry with materialThe combined organic layers were dried over Na2SO4
4. concentrationconcentrated
5. customThe residue was purified by silica gel chromatography
6. washeluted with 20% EtOAc