反应详情

温度

0 °C

To a solution of 0.089 g 5-methyl-thiophene-3-sulfonic acid amide (example 2a) in 4 ml acetonitrile was added at 0° C. 0.094 g phenylchloroformate and 0.127 g triethylamine. The mixture was stirred at 0° C. for 1 h. To the resulting suspension was added 0.127 g 1-(6-amino-4-bromo-pyridin-2-yl)-3-methyl-urea and the mixture was heated to 60° C. for 18 h. The reaction mixture was partitioned between water and ethyl acetate. The phases were separated and the pH of the aqueous phase was adjusted to 2 by addition of 1N hydrochloric acid. The product was extracted with ethyl acetate. The organic phase was washed with water and brine, dried over sodium sulfate and evaporated to yield 0.080 g of the title compound as an orange yellow powder. MS (ISN) M−H+=445.8 and 447.7

1. temperaturethe mixture was heated to 60° C. for 18 h
2. customThe reaction mixture was partitioned between water and ethyl acetate
3. customThe phases were separated
4. additionthe pH of the aqueous phase was adjusted to 2 by addition of 1N hydrochloric acid
5. extractionThe product was extracted with ethyl acetate
6. washThe organic phase was washed with water and brine
7. dry with materialdried over sodium sulfate
8. customevaporated