反应详情

温度

100 °C

A mixture of N-benzyl-2-chloroacetamide (17.8 g), DIPEA (19.5 mL) and 4-fluoro-2-methyl-aniline (10.6 mL) in anhydrous DMF (174 mL) was stirred at 100° C. for 40 hours under a Nitrogen atmosphere. After cooling to r.t., the dark solution was partitioned between AcOEt (200 mL) and water (200 mL). The separated aqueous phase was extracted with further AcOEt (3×200 mL). The combined organic extracts were washed with water (200 mL), dried and concentrated in vacuo. The residue was purified by flash chromatography (CH/AcOEt 2:8) to give a dark solid, which was triturated with CH to give the title compound as a beige solid (16.2 g).

1. temperatureAfter cooling to r.t.
2. customthe dark solution was partitioned between AcOEt (200 mL) and water (200 mL)
3. extractionThe separated aqueous phase was extracted with further AcOEt (3×200 mL)
4. washThe combined organic extracts were washed with water (200 mL)
5. customdried
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography (CH/AcOEt 2:8)
8. customto give a dark solid, which
9. customwas triturated with CH