反应详情

温度

40 °C

Ethyl trifluoroacetate (3.9 g, 0.027 mole) was added over 10 minutes to a warm (40° C.) stirred melt of 5.2 g (0.028 mole) 1-[1,1-dimethylethoxycarbonyl]piperazine. The mixture was heated at 120° C. for 2 hours, cooled to room temperature, treated with 1.0 g (0.007 mole) ethyl trifluoroacetate, and reheated for an additional 2 hours. The mixture was allowed to stand 18 hours at room temperature and then was evaporated in vacuo. The residue was dissolved in ether, passed through an alumina-packed column (2.2×16 cm), the eluent collected, washed with dilute aqueous HCl, dried (MgSO4), filtered, and evaporated in vacuo to yield 6.6 g yellow oil which solidified on standin g Recrystallization from hexane gave 6.0 g of white, crystalline solid, m.p. 66°-68° C. Calc. for C11H17F3N2O3 (282.26): C, 46.81; H, 6.07; N, 9.92. Found: C, 46.76; H, 6.40; N, 10.12.

1. temperatureThe mixture was heated at 120° C. for 2 hours
2. temperaturecooled to room temperature
3. waitto stand 18 hours at room temperature
4. customwas evaporated in vacuo
5. dissolutionThe residue was dissolved in ether
6. customthe eluent collected
7. washwashed with dilute aqueous HCl
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. customevaporated in vacuo