反应详情

温度

50 °C

Dissolve 6-methyl-3′-trifluoromethyl-[2,2′]bipyridinyl-5-carbonitrile (150 mg, 0.570 mmol) and diethyl oxalate (150 mg, 1.03 mmol) in a solution of EtOH (2 mL) and 17% NaOEt in EtOH (0.6 mL, 1.71 mmol). Warm the mixture to 50° C. and stir overnight. Pour the mixture onto ice water (50 mL) and acidify with 3 N HCl. Extract with EtOAc (3×50 mL). Dry the combined organic extracts over Na2SO4 and remove the solvent under reduced pressure. Purify the crude product using silica gel chromatography eluting with EtOAc/hexane (1:1) to yield the title compound. MS 364.11 (M+1).

1. additionPour the mixture onto ice water (50 mL)
2. extractionExtract with EtOAc (3×50 mL)
3. dry with materialDry the combined organic extracts over Na2SO4
4. customremove the solvent under reduced pressure
5. customPurify the crude product
6. washeluting with EtOAc/hexane (1:1)