반응 #171867

반응 방정식

5-(2-(Chloro)-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepin-9-yl)-1-(2,4-difluorophenyl)-1H-1,2,4-triazole

potassium acetate

2-Methylpyridin-3-ylboronic acid

→

474

수율 70.0%

5-(2-(2-methylpyrid-3-yl)-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepin-9-yl)-1-(2,4-difluorophenyl)-1H-1,2,4-triazole

수율 70.0%

용매

acetonitrile

water

반응 조건

후처리

1. 1
   기타The solution was degassed
2. 2
   기타by bubbling with nitrogen for 5 min
3. 3
   기타The reaction was microwaved at 300 watts, 140° C. for 20 minutes
4. 4
   추출extracted with ethyl acetate
5. 5
   농축The combined organics were concentrated
6. 6
   기타purified by reverse phase HPLC

실험 절차

5-(2-(Chloro)-6,7-dihydropyrido[3,2-b]thieno[2,3-d]oxepin-9-yl)-1-(2,4-difluorophenyl)-1H-1,2,4-triazole (50 mg, 0.1 mmol) was dissolved in 1 ml acetonitrile and 1 ml water, with potassium acetate (39.9 mg, 0.406 mmol). The solution was degassed by bubbling with nitrogen for 5 min. 2-Methylpyridin-3-ylboronic acid (21.4 mg, 0.156 mmol) was added, then tetrakis(triphenylphosphine)palladium(0) (19 mg, 0.016 mmol). The reaction was microwaved at 300 watts, 140° C. for 20 minutes, cooled to room temperature, and extracted with ethyl acetate. The combined organics were concentrated and purified by reverse phase HPLC to give 474 (70% yield). MS: (ESI+)=474.0

출처