反应详情

To a solution of 0.030 g (0.0009 mol) of 6-(2,4-dichloro-phenyl)-5-(2-methoxy-ethoxy)-pyrazine-2-carboxylic acid in 2.0 ml dimethylformamide was added at room temperature 0.029 g (0.0018 mol) of 1,1′-carbonyldiimidazole and the mixture was stirred at room temperature for 1 hour. To the resulting brown solution was added 0.020 g (0.0018 mol) 1-amino-2-cyclopropyl-propan-2-ol and the mixture was stirred for 3 hours. The reaction mixture was then partitioned between 10% aqueous citric acid and ethyl acetate. The phases were separated and the organic layer washed with 10% aqueous sodium bicarbonate and brine dried over sodium sulfate and evaporated. The residue was purified by chromatography on silica gel using a gradient of heptane to ethyl acetate to yield 0.021 g of the title compound as colorless oil. MS (ISP) (M+H+)=440.4.

1. stirringthe mixture was stirred for 3 hours
2. customThe reaction mixture was then partitioned between 10% aqueous citric acid and ethyl acetate
3. customThe phases were separated
4. washthe organic layer washed with 10% aqueous sodium bicarbonate and brine
5. dry with materialdried over sodium sulfate
6. customevaporated
7. customThe residue was purified by chromatography on silica gel using a gradient of heptane to ethyl acetate