반응 #680273

반응 방정식

299a

5-Phenylisoxazol-3-amine

3,5-dibromo-1-methylpyridin-2(1H)-one

XantPhos

cesium carbonate

→

299b

수율 122.8%

5-Bromo-1-methyl-3-(5-phenylisoxazol-3-ylamino)pyridin-2(1H)-one

수율 122.8%

용매

1,4-dioxane

반응 조건

후처리

1. 1
   기타A 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and a reflux condenser
2. 2
   기타After three cycles of vacuum/argon flush
3. 3
   온도It was then cooled to room temperature
4. 4
   여과filtered
5. 5
   농축The filtrate was concentrated under reduced pressure
6. 6
   세척the resulting residue was washed with acetonitrile

실험 절차

A 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and a reflux condenser was charged with 1,4-dioxane (40 mL), 299a (640 mg, 4.0 mmol), 3,5-dibromo-1-methylpyridin-2(1H)-one (1.1 g, 4.0 mmol), Pd2(dba)3 (366.8 mg, 0.40 mmol), XantPhos (462.4 mg, 0.80 mmol), and cesium carbonate (2.6 g, 8.0 mmol). After three cycles of vacuum/argon flush, the mixture was heated at 92° C. for 3 hrs. It was then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure and the resulting residue was washed with acetonitrile to afford 299b (1.7 g, 87%). MS-ESI: [M+H]+ 346.0.

출처