反应详情

温度

50 °C

To a solution of (2-chloro-3-trifluoromethyl-benzyl)-(2,2-diphenyl-ethyl)-[3-(3-piperazin-1-yl-phenoxy)-propyl]-amine hydrochloride (114 mg, 0.187 mmol—Example 168) in methanol (15 mL) was treated with bromo-acetic acid methyl ester (57 mg, 0.375 mmol) and diisopropyl-ethyl-amine (48 mg, 0.375 mmol). The resulting solution was heated at 50° C. for 3 hours, cooled to room temperature, and concentrated. The crude material was dissolved in EtOAc and washed with water (1×). The organic layer was then washed with brine (1×), dried over sodium sulfate, and filtered. The EtOAc was concentrated and the sample was dried under vacuum to title compound as an oil (99 mg, 78%). MS(ES) m/e 622.2 ([M−COOCH3]+).

1. temperaturecooled to room temperature
2. concentrationconcentrated
3. dissolutionThe crude material was dissolved in EtOAc
4. washwashed with water (1×)
5. washThe organic layer was then washed with brine (1×)
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationThe EtOAc was concentrated
9. dry with materialthe sample was dried under vacuum to title compound as an oil (99 mg, 78%)