반응 #418447

반응 방정식

6-(2-morpholinoethoxy)-2-bromo-3-phenyl-1H-inden-1-one

Na2CO3

dioxane H2O

→

desired product

수율 64.0%

6-(2-Morpholinoethoxy)-3-phenyl-2-(pyridin-3-yl)-1H-inden-1-one

수율 64.0%

용매

EtOAc

반응 조건

후처리

1. 1
   기타To a microwave reaction vial
2. 2
   기타The reaction
3. 3
   기타vial was placed into a microwave reactor
4. 4
   기타irradiated at 150° C. for 20 min
5. 5
   건조dried over MgSO4
6. 6
   여과The mixture was filtered through a Celite pad
7. 7
   세척while rinsing with EtOAc
8. 8
   농축concentrated in vacuo
9. 9
   기타The residue was purified by prep HPLC (CH3CN/H2O=1:1)

실험 절차

To a microwave reaction vial, 6-(2-morpholinoethoxy)-2-bromo-3-phenyl-1H-inden-1-one (1.0 g, 2.5 mmol) obtained in Step 6,3-pyridinylboronic acid (470 mg, 3.8 mmol, 1.5 eq), Pd(PPh3)4 (180 mg, 6 mol %), Na2CO3 (800 mg, 3.0 eq), and dioxane/H2O (4:1, 5 mL) were sequentially charged. The reaction vial was placed into a microwave reactor and irradiated at 150° C. for 20 min. After cooling to room temperature, the reaction was diluted with EtOAc and dried over MgSO4. The mixture was filtered through a Celite pad while rinsing with EtOAc and then concentrated in vacuo. The residue was purified by prep HPLC (CH3CN/H2O=1:1) to afford the desired product (640 mg, 64%).

출처