Reaktion #84372

Reaktionsgleichung

thiomorpholine

Et3N

3,4-difluoronitrobenzene

→

title compound

Ausbeute 72.2%

4-(2-fluoro-4-nitrophenyl)thiomorpholine

Ausbeute 72.2%

Lösungsmittel

EtOAc

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONUpon the end of addition the reaction mixture
2. 2
   Sonstigesolid was precipitated out
3. 3
   FiltrationThe mixture was filtered
4. 4
   WaschenThe filter cake was washed with an appropriate amount of water
5. 5
   Sonstigedried in vacuo
6. 6
   Sonstigeto obtain the 1st crop of product
7. 7
   ExtraktionThe filtrate was extracted with EtOAc
8. 8
   TrocknenThe combined organic phases were dried over anhydrous Na2SO4
9. 9
   Einengenconcentrated in vacuo
10. 10
    Sonstigeto obtain the 2nd crop of product

Vorschrift

To a solution of thiomorpholine (3.57 g, 34.56 mmol) and Et3N (3.50 g, 34.56 mmol) in EtOAc was added 3,4-difluoronitrobenzene (5.00 g, 31.43 mmol) dropwise over a period of 30 min in an ice bath. Upon the end of addition the reaction mixture was warmed to rt slowly, and solid was precipitated out. The mixture was filtered. The filter cake was washed with an appropriate amount of water, dried in vacuo to obtain the 1st crop of product. The filtrate was extracted 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 (5.50 g, 72%).

Quelle