반응 #40842

반응 방정식

Compound 87

3-(Methylsulfonyl)-5,6-diphenyl-1,2,4-triazine

ethyl acetoacetate

NaH

3-(methylsulfonyl)-5,6-diphenyl-1,2,4-triazine

3-(Methylsulfonyl)-5,6-diphenyl-1,2,4-triazine

→

title compound

Ethyl 2-(5,6-Diphenyl-1,2,4-triazin-3-yl)acetate

용매

THF

THF

반응 조건

후처리

1. 1
   기타The reaction was then quenched with water
2. 2
   추출The product was extracted with ethyl acetate
3. 3
   세척The organic layer was washed with water, and brine
4. 4
   건조dried over Na2SO4
5. 5
   농축The filtered solvent was concentrated in vacuo
6. 6
   기타the residue was purified by silica gel chromatography (20% ethyl acetate in hexane)

실험 절차

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.

출처