反应详情

温度

50 °C

A mixture of N-methoxy-N-methyl-2,4-dimethoxybenzamide (7.2 g, 32 mmol), prepared as in Example 4, N-chlorosuccinimide (4.8 mL, 36 mmol) and acetonitrile (100 mL) was heated 16 hours at 50° C. The mixture was concentrated and the residue was partitioned between ethyl acetate (300 mL) and saturated sodium bicarbonate (150 mL). The mixture was filtered and the organic layer was separated, washed with water (4×) and brine (1×), dried (K2CO3), filtered through a short column of silica-gel and concentrated to give N-methoxy-N-methyl-5-chloro-2,4-dimethoxybenzamide (5.3 g, 20 mmol), m.p. 97°-99° C.

1. concentrationThe mixture was concentrated
2. customthe residue was partitioned between ethyl acetate (300 mL) and saturated sodium bicarbonate (150 mL)
3. filtrationThe mixture was filtered
4. customthe organic layer was separated
5. washwashed with water (4×) and brine (1×)
6. dry with materialdried (K2CO3)
7. filtrationfiltered through a short column of silica-gel
8. concentrationconcentrated