反应详情

温度

0 °C

To a mixture of 0.089 ml (1.1 mmol) N,N-dimethylformamide and 38 mg (0.56 mmol) imidazole 0.071 ml (0.56 mmol) trimethylchlorosilane were added dropwise at room temperature. The reaction mixture was cooled to 0° C., and 0.10 g (0.19 mmol) N-(3,5-bis-trifluoromethyl-benzyl)-N-methyl-6-piperazin-1-yl-4-o-tolyl-nicotinamide (Example 53) were added. The ice-water bath was removed and the mixture stirred over night. The reaction was quenched with a mixture of 2 ml 1 N aqueous hydrochloric acid solution and 4 ml water, and the mixture was extracted with ethyl acetate. The combined extracts were dried with sodium sulfate and concentrated. Flash column chromatography afforded 81 mg (82%) of the title compound as a white solid.

1. additionwere added dropwise at room temperature
2. customThe ice-water bath was removed
3. customThe reaction was quenched with a mixture of 2 ml 1 N aqueous hydrochloric acid solution and 4 ml water
4. extractionthe mixture was extracted with ethyl acetate
5. dry with materialThe combined extracts were dried with sodium sulfate
6. concentrationconcentrated