Reaktion #75119

Reaktionsgleichung

1-chloro-2-nitro-4-(trifluoromethyl)benzene

3-amino-1-propanol

→

3-{[2-nitro-4-(trifluoromethyl)phenyl]amino}-1-propanol

Ausbeute 100.0%

Lösungsmittel

butanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturtill reflux
3. 3
   workup.STIRRINGStirring
4. 4
   Temperaturat reflux
5. 5
   TemperaturThe reaction mixture is cooled
6. 6
   Sonstigeevaporated
7. 7
   workup.ADDITIONWater is added to the residue
8. 8
   ExtraktionThe product is extracted with methylbenzene
9. 9
   SonstigeThe extract is dried
10. 10
    Filtrationfiltered
11. 11
    Sonstigeevaporated
12. 12
    SonstigeThe solid residue is crystallized from petroleumether
13. 13
    FiltrationThe product is filtered off
14. 14
    Sonstigedried

Vorschrift

A mixture of 100 parts of 1-chloro-2-nitro-4-(trifluoromethyl)benzene, 90 parts of 3-amino-1-propanol and 200 parts of butanol is stirred and heated till reflux. Stirring at reflux is continued overnight. The reaction mixture is cooled and evaporated. Water is added to the residue and the whole is acidified with a hydrochloric acid solution. The product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The solid residue is crystallized from petroleumether. The product is filtered off and dried, yielding 141 parts (100%) of 3-{[2-nitro-4-(trifluoromethyl)phenyl]amino}-1-propanol.

Quelle