反应详情

To an ice-cooled solution of 6-methylpyridin-2-amine [CAS 1824-81-3] (5.22 g, 44.08 mmol) in 350 mL anhydrous THF was added diisopropylethylamine (15.36 mL, 88.16 mmol). Chloro(phenyl)acetyl chloride [CAS 2912-62-1] (10.0 g, 52.9 mmol) was added dropwise and the resulting mixture was stirred for 1 h while cooling was maintained. The mixture was partitioned between ethyl acetate and water and the organic phase was washed with brine. The organic phase was filtered through a Whatman filter and the volatile components were removed by the use of a rotary evaporator to give title compound (14.3 g) in ˜80% purity (LC-MS). The crude material was forwarded directly to the next step.

1. temperaturewhile cooling
2. temperaturewas maintained
3. customThe mixture was partitioned between ethyl acetate and water
4. washthe organic phase was washed with brine
5. filtrationThe organic phase was filtered through a Whatman
6. filtrationfilter
7. customthe volatile components were removed by the use of a rotary evaporator