反応 #75119

反応方程式

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

3-amino-1-propanol

→

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

収率 100.0%

溶媒

butanol

反応条件

後処理

1. 1
   温度heated
2. 2
   温度till reflux
3. 3
   workup.STIRRINGStirring
4. 4
   温度at reflux
5. 5
   温度The reaction mixture is cooled
6. 6
   その他evaporated
7. 7
   workup.ADDITIONWater is added to the residue
8. 8
   抽出The product is extracted with methylbenzene
9. 9
   その他The extract is dried
10. 10
    ろ過filtered
11. 11
    その他evaporated
12. 12
    その他The solid residue is crystallized from petroleumether
13. 13
    ろ過The product is filtered off
14. 14
    その他dried

実験手順

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.

出典