反应详情

温度

65 °C

To a solution of methyl 5-tosyl-5H-pyrrolo[2,3-b]pyrazine-2-carboxylate (2.5 g, 7.5 mmol) in 1,4-dioxane (50 mL) was added aqueous 6 N HCl (50.0 mL, 1650 mmol) and the reaction mixture was stirred at about 65° C. for about 5 h and at room temperature for about 72 h. The mixture was re-heated to about 60° C. for about 3 h, and stirred at room temperature for about 48 h. The mixture was re-heated to about 65° C. for about 2 h and then cooled to room temperature. An insoluble bright yellow residue was removed by filtration and the organic solvent was removed under reduced pressure to give a precipitate that was collected and dried to give 5-tosyl-5H-pyrrolo[2,3-b]pyrazine-2-carboxylic acid hydrochloride (1.92 g, 72%) as a tan solid: LC/MS (Table 2, Method a) Rt=1.48 min; MS m/z: 352 (M−H)−.

1. temperatureThe mixture was re-heated to about 60° C. for about 3 h
2. stirringstirred at room temperature for about 48 h
3. temperatureThe mixture was re-heated to about 65° C. for about 2 h
4. temperaturecooled to room temperature
5. customAn insoluble bright yellow residue was removed by filtration
6. customthe organic solvent was removed under reduced pressure
7. customto give a precipitate that
8. customwas collected
9. customdried