반응 #84366

반응 방정식

morpholine

Et3N

3,4-difluoronitrobenzene

→

title compound

수율 99.0%

4-(2-fluoro-4-nitrophenyl)morpholine

수율 99.0%

용매

EtOAc

반응 조건

후처리

1. 1
   여과filtered
2. 2
   세척The filter cake was washed with water
3. 3
   기타dried in vacuo
4. 4
   기타to obtain the 1st crop of product
5. 5
   기타The organic phase was separated from the filtrate
6. 6
   세척the water phase was washed with EtOAc
7. 7
   건조The combined organic phases were dried over anhydrous Na2SO4
8. 8
   농축concentrated in vacuo
9. 9
   기타to obtain the 2nd crop of product

실험 절차

To a solution of morpholine (12.04 g, 0.14 mol) and Et3N (13.97 g, 0.14 mol) in EtOAc was added 3,4-difluoronitrobenzene (20.0 g, 0.13 mol) dropwise in an ice bath. The reaction mixture was warmed to rt slowly, stirred at rt overnight, and then filtered. The filter cake was washed with water, dried in vacuo to obtain the 1st crop of product. The organic phase was separated from the filtrate, and the water phase was washed with EtOAc. The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo to obtain the 2nd crop of product. The solids of 1st crop and 2nd crop were combined to give the title compound as a yellow solid (28.0 g, 99%).

출처