反应详情

温度

100 °C

To a solution of 3-amino-5-chloro-6-methoxy-4-methyl-thieno[2,3-b]pyridine-2-carboxylic acid cyclopropylamide (5.0 g, 16.04 mmol) in DMF (45 ml) is added solid 95% sodium thiomethoxide (1.30 g, 17.64 mmol). The reaction vessel is sealed and heated at 100° C. for 5 hours. The reaction is cooled to room temperature and quenched by the addition of water (75 ml). The mixture is acidified to pH2 by the addition of 5N HCl. Gradually, a thick, white precipitate is formed, which is stirred at 0° C. for 10 minutes, then collected by filtration. The solid is dried in the vacuum oven overnight at 60° C. to afford the title compound as a white solid (4.13 g, 86%). Mass (m/z): 298.0 (M++1).

1. customThe reaction vessel is sealed
2. temperatureThe reaction is cooled to room temperature
3. customquenched by the addition of water (75 ml)
4. additionThe mixture is acidified to pH2 by the addition of 5N HCl
5. customGradually, a thick, white precipitate is formed
6. filtrationcollected by filtration
7. customThe solid is dried in the vacuum oven overnight at 60° C.