反应详情

温度

25 °C

A mixture of 5-bromopyridin-2-amine (14.7 g, 85.0 mmol) and ethoxycarbonyl isothiocyanate (11.1 g, 10.0 ml, 85.0 mmol) in dioxane (300 ml) was stirred for 18 hours at 25° C. under nitrogen atmosphere. The solvent was evaporated under reduced pressure, the solid yellow residue was diluted with ethyl acetate and washed with water and brine, the organic layer was separated, dried over magnesium sulfate, filtrated and evaporated to dryness. 26.2 g (quant.) light yellow solid. Mp.: 159-161° C. MS: m/z=304.0/305.9 (M+H+).

1. customThe solvent was evaporated under reduced pressure
2. additionthe solid yellow residue was diluted with ethyl acetate
3. washwashed with water and brine
4. customthe organic layer was separated
5. dry with materialdried over magnesium sulfate
6. filtrationfiltrated
7. customevaporated to dryness