反应详情

To a solution of 3-methyl-1H-pyrazole-4-carbaldehyde (273 mg, 2.48 mmol) in anhydrous DMF (5 mL) was added 60% NaH (130 mg, 3.25 mmol) at 0° C. After being stirred for 30 min at room temperature, it was cooled to 0° C. To this, was added intermediate 5 (542 mg, 1.65 mmol) and then stirred for 6 hours at 60° C. Quenching the reaction by addition of ice and 20 mL of water resulted precipitation of brown solids. The resulted solids were collected by filtration, rinsed with water and the dried in vacuo to provide the desired intermediate 6 as a brown solid (424 mg, 80%); MS (ESI) m/z 403 [M+H]+.

1. temperatureit was cooled to 0° C
2. stirringstirred for 6 hours at 60° C
3. customQuenching
4. customthe reaction
5. customresulted
6. customprecipitation of brown solids
7. filtrationThe resulted solids were collected by filtration
8. washrinsed with water
9. customthe dried in vacuo