反应详情

温度

60 °C

To a suspension of NaH (41 mg, 1.61 mmol) in THF (2 ml) at 0° C. was added ethyl acetoacetate (105 mg. 0.80 mmol) dropwise. After the mixture was stirred for 15 min, a solution of 3-(methylsulfonyl)-5,6-diphenyl-1,2,4-triazine (Compound 87) (250 mg, 0.80 mmol) in THF (3 ml) was cannulated into the solution, and the resulting solution was heated to 60° C. for 2 hours. The reaction was then quenched with water. The product was extracted with ethyl acetate. The organic layer was washed with water, and brine, and dried over Na2SO4. The filtered solvent was concentrated in vacuo, and the residue was purified by silica gel chromatography (20% ethyl acetate in hexane) to give title compound as a solid.

1. customThe reaction was then quenched with water
2. extractionThe product was extracted with ethyl acetate
3. washThe organic layer was washed with water, and brine
4. dry with materialdried over Na2SO4
5. concentrationThe filtered solvent was concentrated in vacuo
6. customthe residue was purified by silica gel chromatography (20% ethyl acetate in hexane)