反应详情

温度

60 °C

[3-(4-morpholinyl)-5-(trifluoromethyl)phenyl]-carbamic acid, 1,1-dimethylethyl ester (Example 90b; 1.7 g, 5 mmol) is treated with a solution of hydrogen chloride in isopropanol (30 mL of 4 M) and heated at 60° C. for 5 h. The solvent is evaporated off under reduced pressure and the residue is treated with aqueous sodium hydrogen carbonate solution (80 mL) and extracted with ethyl acetate (3×80 mL). The combined extracts are washed with brine (2×50 mL), dried (MgSO4) and the solvent is evaporated off under reduced pressure to give the crude product which is purified by recrystallisation from ether-hexane to afford the title compound as yellow crystalline solid, m.p. 96-97° C.

1. customThe solvent is evaporated off under reduced pressure
2. additionthe residue is treated with aqueous sodium hydrogen carbonate solution (80 mL)
3. extractionextracted with ethyl acetate (3×80 mL)
4. washThe combined extracts are washed with brine (2×50 mL)
5. dry with materialdried (MgSO4)
6. customthe solvent is evaporated off under reduced pressure
7. customto give the crude product which
8. customis purified by recrystallisation from ether-hexane