反应详情

温度

-15 °C

Iso-butylchloroformate (60 μL, 0.46 mmol) was added to a stirred solution of N-(2-{[3-chloro-4-(2-methylbenzoyl)phenyl]amino}phenyl)-succinamic acid (200 mg, 0.46 mmol) (disclosed in WO 01/05746) and 4-methylmorpholine (51 μL, 0.46 mmol) in THF (5.0 mL) at −15° C. After 5 min at 0° C. the reaction mixture was cooled to −15° C. and a solution of ethyl diisopropyl amine (65 μL, 0.46 mmol) in THF (5.0 mL) was added. The resulting reaction mixture was kept at 0° C. for 1 h. The reaction mixture was stirred for 16 h at RT and then poured into a mixture of 1 M HCl(aq) and EtOAc. The organic phase was washed with more HCl(aq)(×2). The organic phase was washed with brine, dried (MgSO4), filtered and concentrated in vacuo. The crude product was purified by flash chromatography using petroleum ether/EtOAc 1:2 as the eluent to afford the title compound as an oil.

1. customThe resulting reaction mixture
2. washThe organic phase was washed with more HCl(aq)(×2)
3. washThe organic phase was washed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe crude product was purified by flash chromatography