反应详情

温度

0 °C

To a solution of methyl 2-(2-fluoro-4-iodophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylate (0.500 g, 1.20 mmol) in THF (60 mL) was added O-(2-vinyloxy-ethyl)-hydroxylamine (0.149 g, 1.44 mmol). The solution was cooled to 0° C. and lithium bis(trimethylsilyl)amide (4.81 ml, 4.81 mmol) (1 M solution in hexanes) was added dropwise. The reaction mixture was warmed to room temperature. After stirring for 10 minutes the reaction mixture was quenched by the addition of 1 M HCl and partitioned between EtOAc and saturated NaCl. The layers were separated and the organic layer was dried (Na2SO4) and concentrated under reduced pressure to yield a crude yellow solid that was used without purification in the next step.

1. temperatureThe reaction mixture was warmed to room temperature
2. customwas quenched by the addition of 1 M HCl
3. custompartitioned between EtOAc and saturated NaCl
4. customThe layers were separated
5. dry with materialthe organic layer was dried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customto yield a crude yellow solid that
8. customwas used without purification in the next step