反应详情

温度

-78 °C

4-Iodo-2-methylaniline (233 mg, 1.00 mmol) and 3-fluoropyridine-4-carboxylic acid (141 mg, 1.00 mmol) were dissolved in dry THF (6.0 ml) under argon and the mixture was cooled to −78° C. A solution of LiHMDS (1.0M in THF, 3.5 ml) was added and the reaction mixture was allowed to warm to ambient temperature. After 36 h the reaction was quenched by adding solid NH4Cl. After filtration the volatiles were removed in vacuo and the crude material was purified by flash chromatography using silica gel and a gradient of 0-10% methanol in DCM as eluent to give 208 mg (588 μmol; 59% yield) of pure desired product.

1. temperatureto warm to ambient temperature
2. customAfter 36 h the reaction was quenched
3. additionby adding solid NH4Cl
4. filtrationAfter filtration the volatiles
5. customwere removed in vacuo
6. customthe crude material was purified by flash chromatography