HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus sulfide (P2S5) → HCID 178446234, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 6-(Cyclohexylmethyl)-1-(1-ethylpropyl)-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one | HCID 135422930 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 178446234 | HCID 178446234 | — |
Reaction Steps
74 mg (0.33 mmol, 2 equiv.) of diphosphorus pentasulfide are added to a solution of 50 mg (0.17 mmol) of 6-(cyclohexylmethyl)-1-(1-ethylpropyl)-1,5-dihydro-4H-pyrazolo[3,4-d]pyrimidin-4-one (Example 3) in 1 ml of pyridine at room temperature, and the mixture is then stirred under reflux overnight. After cooling, the reaction solution is mixed with 20 ml of ice-cold 2.5% strength sodium bicarbonate solution and extracted three times with ethyl acetate. The combined organic phases are washed with saturated brine, dried over sodium sulfate and concentrated in vacuo. The crude product is purified by preparative HPLC.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08039477B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-e579fdb6e87d4cab8616ccdad0e88e82 |
| Source note | uspto-grants-2011_10 |