反应详情

2-Chloro-3-nitro-6-trifluoromethyl-pyridin-4-ylamine (2.2 g, 9.1 mmol) was stirred in 2-MeTHF (20 ml) and triethylamine added (1.52 ml, 10.9 mmol). The solution was cooled in an ice bath to ˜5° C. before the dropwise addition of ethyl chloroformate (1.04 ml, 10.9 mmol), the solution warmed to ambient temperature and left to stir under a nitrogen atmosphere for 16 h. 20 ml EtOAc and 10 ml H20 were added and the phases separated, washed with a additional 2×10 ml sat'd brine solution. The organic extract was dried over MgSO4, concentrated in vacuo and preabsorbed onto a silica column. Elution with Hept:EtOAc, 9:1 gave 2.1 g of the title compound as a white solid.

1. waitleft
2. customthe phases separated
3. washwashed with a additional 2×10 ml
4. extractionThe organic extract
5. dry with materialwas dried over MgSO4
6. concentrationconcentrated in vacuo
7. custompreabsorbed onto a silica column
8. washElution with Hept