反应详情

温度

0 °C

A mixture of 3-benzyloxy-2,2-dimethylpropionic acid (1.6 g, 7.5 mmol), benzene (10 mL) and DMF (2 drops) was cooled to between 0° and 5° C. and then oxalyl chloride (0.98 mL, 11.2 mmol) was added slowly. The mixture was stirred 1.5 hours at between 20° and 25° C. and concentrated. The residue was dissolved in benzene (10 mL) and the solution reconcentrated (repeated once). The residue then was dissolved in benzene (6 mL) and the solution was cooled to 0° C. and added to a cold (0° C.) mixture of 1-[2-(2,2,2-trifluoroethoxy)phenyl]piperazine (2.1 g, 8.24 mmol) and benzene (6 mL). The mixture was cooled 15 hours at 0° C. and then triethylamine (3 mL, 21.3 mmol) was added. The mixture was stirred an additional 20 minutes, diluted with 10 mL of saturated sodium carbonate and extracted with methylene chloride (3×15 mL). The combined extracts were washed with water (1×10 mL), dried (MgSO4) and concentrated. The residue was purified by chromatography on silica gel eluting with hexanes/ethyl acetate (8:2) to give 3-benzyloxy-2,2-dimethyl-1-{4-[2-(2,2,2-trif-luoroethoxy)phenyl]piperazin-1-yl}-1-propanone (2.8 g, 6.4 mol).

1. temperaturewas cooled to between 0° and 5° C.
2. concentrationconcentrated
3. dissolutionThe residue was dissolved in benzene (10 mL)
4. dissolutionThe residue then was dissolved in benzene (6 mL)
5. temperatureThe mixture was cooled 15 hours at 0° C.
6. stirringThe mixture was stirred an additional 20 minutes
7. extractionextracted with methylene chloride (3×15 mL)
8. washThe combined extracts were washed with water (1×10 mL)
9. dry with materialdried (MgSO4)
10. concentrationconcentrated
11. customThe residue was purified by chromatography on silica gel eluting with hexanes/ethyl acetate (8:2)