反应详情

温度

50 °C

To a mixture of methyl 2-(4-amino-2-chlorophenyl)acetate (step 4, 2.6 g, 13.0 mmol) and 4,6-Dimethyl-3-nitro-2-pyridine (step 2 of Example 1, 2.4 g, 13.0 mmol) in DMSO was added diisopropylethylamine. The resulting mixture was stirred for 9 h at 50° C. To the mixture was poured into water and extracted with ethyl acetate (3×30 ml). The organic layer was washed with brine, dried (MgSO4) and concentrated to give a brown oil. This was purified by SiO2 column chromatography with developing hexane/ethyl acetate (10/1) to give 1.4 g (29%) of title compound as yellow solid.

1. extractionextracted with ethyl acetate (3×30 ml)
2. washThe organic layer was washed with brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customto give a brown oil
6. customThis was purified by SiO2 column chromatography with developing hexane/ethyl acetate (10/1)