反应详情

温度

150 °C

A mixture of N-[6-bromo-7-methyl-8-(3-trifluoromethyl-phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-yl]-acetamide (Int. 18, 330 mg, 0.80 mmol), hydroxylamine hydrochloride (112 mg, 1.60 mmol), trans-bis(acetato)bis[o-(di-o-tolylphosphino)benzyl]dipalladium(II) (38 mg, 0.04 mmol), tri-tert-butylphosphonium tetrafluoroborate, (22 mg, 0.08 mmol), 1,8-diazabicyclo[5.4.0]undec-7-ene (0.12 mL, 0.80 mmol), N,N-diisopropylethylamine, (0.28 mL, 1.60 mmol) and molybdenum hexacarbonyl (106 mg, 0.40 mmol) in dioxane (2 mL) was heated at 150° C. for 20 minutes using microwave irradiation. The reaction mixture was cooled and filtered through Celite®. The solvent was concentrated in vacuo and the residue purified by chromatography eluting with a gradient of 0-100% cyclohexane in EtOAc and then with 10% MeOH in EtOAc to afford the title compound as a beige foam (105 mg).

1. custommicrowave irradiation
2. temperatureThe reaction mixture was cooled
3. filtrationfiltered through Celite®
4. concentrationThe solvent was concentrated in vacuo
5. customthe residue purified by chromatography
6. washeluting with a gradient of 0-100% cyclohexane in EtOAc