反应详情

温度

0 °C

5-Bromo-1,6-dihydro-6-oxo-2-(trifluoromethyl)-3-pyridinecarboxylic acid ethyl ester (CAS Registry No. 862111-61-3) (5.0 g, 16 mmol) was dissolved in tetrahydrofuran (80 mL). To the solution were added trifluoroethanol (1.37 mL, 19 mmol), triphenylphosphine (5.0 g, 19 mmol) and diethyl azodicarboxylate (3.7 mL, 19 mmol) at 0° C. The mixture was stirred for 30 min at 0° C. and for 6 h at room temperature. The solvent was removed in vacuo and the residue dissolved in dichloromethane and washed with water. Organic phases were pooled, dried with MgSO4 and concentrated in vacuo. The residue was purified by chromatography on silica gel with dichloromethane:heptane 1:2 to yield the product as white solid, MS (ISP) 397 (M+H)+.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue dissolved in dichloromethane
3. washwashed with water
4. dry with materialdried with MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by chromatography on silica gel with dichloromethane:heptane 1:2