反应详情

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.

1. concentrationThe mixture was concentrated
2. additiontreated with 20 ml water, 20 ml 2M Na2CO3
3. extractionextracted with 50 ml EtOAc
4. washThe organic phase was washed with 30 ml saturated NaCl
5. extractionextracted with 50 ml EtOAc
6. dry with materialThe combined organic phases were dried with MgSO4
7. customevaporated