تفاعل #84366

معادلة التفاعل

morpholine

Et3N

3,4-difluoronitrobenzene

→

title compound

المردود 99.0%

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

المردود 99.0%

المذيبات

EtOAc

ظروف التفاعل

المعالجة

1. 1
   ترشيحfiltered
2. 2
   غسيلThe filter cake was washed with water
3. 3
   أخرىdried in vacuo
4. 4
   أخرىto obtain the 1st crop of product
5. 5
   أخرىThe organic phase was separated from the filtrate
6. 6
   غسيلthe water phase was washed with EtOAc
7. 7
   تجفيفThe combined organic phases were dried over anhydrous Na2SO4
8. 8
   تركيزconcentrated in vacuo
9. 9
   أخرىto obtain the 2nd crop of product

الإجراء التجريبي

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%).

المصدر