تفاعل #40842

معادلة التفاعل

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

المذيبات

THF

THF

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction was then quenched with water
2. 2
   استخلاصThe product was extracted with ethyl acetate
3. 3
   غسيلThe organic layer was washed with water, and brine
4. 4
   تجفيفdried over Na2SO4
5. 5
   تركيزThe filtered solvent was concentrated in vacuo
6. 6
   أخرىthe residue was purified by silica gel chromatography (20% ethyl acetate in hexane)

الإجراء التجريبي

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.

المصدر