반응 #60933

반응 방정식

4-(2-Fluoro-4-trifluoromethyl-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

HCl

→

title compound

수율 95.0%

1-(2-Fluoro-4-trifluoromethyl-phenyl)-piperazine

수율 95.0%

용매

dioxane

dioxane

반응 조건

후처리

1. 1
   농축The mixture was concentrated
2. 2
   workup.ADDITIONtreated with 20 ml water, 20 ml 2M Na2CO3
3. 3
   추출extracted with 50 ml EtOAc
4. 4
   세척The organic phase was washed with 30 ml saturated NaCl
5. 5
   추출extracted with 50 ml EtOAc
6. 6
   건조The combined organic phases were dried with MgSO4
7. 7
   기타evaporated

실험 절차

A mixture of 3.11 g (9 mmol) 4-(2-Fluoro-4-trifluoromethyl-phenyl)-piperazine-1-carboxylic acid tert-butyl ester in 20 ml dioxane was treated with 8.93 ml 4N HCl in dioxane for 2 h at 80° C. The mixture was concentrated and treated with 20 ml water, 20 ml 2M Na2CO3 and extracted with 50 ml EtOAc. The organic phase was washed with 30 ml saturated NaCl. All aqueous phases were combined and extracted with 50 ml EtOAc. The combined organic phases were dried with MgSO4 and evaporated to yield 2.1 g (95%) of the title compound as brownish crystals.

출처