反应详情

温度

0 °C

To a suspension of 3-amino-6-bromo-W-(3,3,3-trifluoro-2-hydroxy-2-methylpropanoyl)-5-(trifluoromethyl)picolinohydrazide (step 1) (4 g, 9.11 mmol) in DCM (60 ml), triethylamine (1.270 ml, 9.11 mmol) was added to give a yellow solution. The solution was cooled to 0° C. (ice bath) and treated with triisopropylsilyl trifluoromethanesulfonate (4.94 ml, 18.22 mmol). The reaction mixture was stirred at 0° C. for 1 hour and allowed to warm to RT and stirred for 3 days. The reaction mixture was partitioned between DCM (100 ml) and water (100 ml), phases shaken and separated. The organic portion was washed with brine (100 ml), dried (MgSO4) and concentrated in vacuo. The resulting oil was purified by chromatography on silica eluting with 0-30% DCM in iso-hexane to afford the title compound; LC-MS Rt=1.58 min [M+H]+ 595/597 Method 2minLC_v003.

1. additionwas added
2. customto give a yellow solution
3. temperatureto warm to RT
4. stirringstirred for 3 days
5. customThe reaction mixture was partitioned between DCM (100 ml) and water (100 ml), phases
6. stirringshaken
7. customseparated
8. washThe organic portion was washed with brine (100 ml)
9. dry with materialdried (MgSO4)
10. concentrationconcentrated in vacuo
11. customThe resulting oil was purified by chromatography on silica eluting with 0-30% DCM in iso-hexane