反应详情

温度

100 °C

To a solution of 2-methyl-2-(3-nitro-phenyl)-propionic acid 2-bromo-ethyl ester (1.5 g, 4.74 mmol) in DMF (8 mL) was added sodium iodide (0.73 g, 4.87 mmol) and heated at 100° C. for 1 h. 2-Isopropyl-imidazole (2.15 g, 19.5 mmol) and triethylamine (2 mL, 14.6 mmol) were added and then refluxed for 4 h. The reaction was diluted with water and extracted with DCM. The organic layer was washed thoroughly with water, dried over sodium sulfate and evaporated to obtain crude compound. Purification by column chromatography on silica gel (60-120 mesh), eluting with 30% ethyl acetate/hexane gave 2-methyl-2-(3-nitro-phenyl)-propionic acid 2-(2-isopropyl-imidazol-1-yl)-ethyl ester (320 mg, 20%) as a solid.

1. temperaturerefluxed for 4 h
2. extractionextracted with DCM
3. washThe organic layer was washed thoroughly with water
4. dry with materialdried over sodium sulfate
5. customevaporated
6. customto obtain crude compound
7. customPurification by column chromatography on silica gel (60-120 mesh)
8. washeluting with 30% ethyl acetate/hexane