反应详情

温度

70 °C

To a solution of 6-bromo-4-[5-(chloromethyl)-1,3,4-oxadiazol-2-yl]-1-(phenylsulfonyl)-1H-indazole (200 mg, 0.441 mmol) in acetonitrile (2 ml) was added 2,2-dimethylmorpholine (102 mg, 0.882 mmol, available from Chembridge Corporation) and the mixture heated at 70° C. for 18 hr. The mixture was cooled to room temperature and a further portion of 2,2-dimethylmorpholine (102 mg, 0.882 mmol), DIPEA (0.154 mL, 0.882 mmol) and sodium iodide (66.1 mg, 0.441 mmol) were added. The mixture was then heated again at 70° C. for 2 hours. The mixture was cooled to room temperature, diluted with DCM and washed with water. The organic layer was separated through a hydrophobic frit and the solvent removed in vacuo. The resulting yellow oil was dried in a vacuum oven at 60° C. overnight to give a pale yellow solid, which was dissolved in DCM (10 ml) and washed with dilute HCl (10 ml) followed by water (10 ml), separating the layers using a hydrophobic frit. The DCM was removed in vacuo to give the title compound as a cream solid (214 mg).

1. temperatureThe mixture was cooled to room temperature
2. temperatureThe mixture was then heated again at 70° C. for 2 hours
3. temperatureThe mixture was cooled to room temperature
4. washwashed with water
5. customThe organic layer was separated through a hydrophobic frit
6. customthe solvent removed in vacuo
7. customThe resulting yellow oil was dried in a vacuum oven at 60° C. overnight
8. customto give a pale yellow solid, which
9. washwashed with dilute HCl (10 ml)
10. customseparating the layers
11. customThe DCM was removed in vacuo