HCID 18944693, compound → HCID 86658773, compound

Temperature

60 °C

Into a 100-mL 3-necked round-bottom flask, was placed a solution of 4,6-dichloro-3-ethyl-1-phenyl-1H-pyrazolo[3,4-d]pyrimidine (300 mg, 1.03 mmol, 1.00 equiv) in dichloromethane (10 mL) at room temperature. To the resulting mixture was then added Zn (400 mg, 6.15 mmol, 6.00 equiv), in portions at room temperature, followed by NH3/NaCl (10 mL), in portions at room temperature. The resulting solution was stirred overnight at 60° C. The solids were filtered out. The resulting solution was extracted with dichloromethane (2×50 mL) and the organic layers combined. The resulting mixture was washed with sodium chloride (3×50 mL). The resulting mixture was dried over anhydrous sodium sulfate and the solids were filtered out. The resulting mixture was concentrated under vacuum to yield 6-chloro-3-ethyl-1-phenyl-1H-pyrazolo[3,4-d]pyrimidine as a yellow solid. MS (m/z): 258 [MH+].

1. customInto a 100-mL 3-necked round-bottom flask, was placed
2. customat room temperature
3. customat room temperature
4. filtrationThe solids were filtered out
5. extractionThe resulting solution was extracted with dichloromethane (2×50 mL)
6. washThe resulting mixture was washed with sodium chloride (3×50 mL)
7. dry with materialThe resulting mixture was dried over anhydrous sodium sulfate
8. filtrationthe solids were filtered out
9. concentrationThe resulting mixture was concentrated under vacuum

ORD record

ord-8af975904c484c3eb6fec113cb69abc1

Source dataset

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08822447B2