反应详情

Into a 100-mL 3-necked round-bottom flask, was placed a solution of 6-chloro-3-ethyl-1-phenyl-1H-pyrazolo[3,4-d]pyrimidine (420 mg, 1.63 mmol, 1.00 equiv) in C7H8 (15 mL) at room temperature. To the resulting mixture was then added 1-(1-benzhydrylazetidin-3-yl)piperazine (500 mg, 1.63 mmol, 1.00 equiv), in portions at room temperature, followed by triethylamine (490 mg, 4.85 mmol, 3.00 equiv), in portions at room temperature. The resulting solution was heated to reflux overnight. The resulting mixture was concentrated under vacuum. The residue was dissolved in DCM (20 mL). The resulting mixture was washed with sodium chloride (2×15 mL). The resulting mixture was concentrated under vacuum. The resulting mixture was washed with methanol (1×5 mL). The solids were collected by filtration to yield 6-(4-(1-benzhydrylazetidin-3-yl)piperazin-1-yl)-3-ethyl-1-phenyl-1H-pyrazolo[3,4-d]pyrimidine as a yellow solid. MS (m/z): 530 [MH+].

1. customInto a 100-mL 3-necked round-bottom flask, was placed
2. customat room temperature
3. customat room temperature
4. temperatureThe resulting solution was heated
5. temperatureto reflux overnight
6. concentrationThe resulting mixture was concentrated under vacuum
7. dissolutionThe residue was dissolved in DCM (20 mL)
8. washThe resulting mixture was washed with sodium chloride (2×15 mL)
9. concentrationThe resulting mixture was concentrated under vacuum
10. washThe resulting mixture was washed with methanol (1×5 mL)
11. filtrationThe solids were collected by filtration