HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → HCID 58305976, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2-[1-(Cyclopropylmethyl)piperidin-4-yl]-7-(2,4-dichlorophenyl)[1,2,4]triazolo[1,5-c]pyrimidin-5(6H)-one hydrochloride | HCID 136337814 | — |
| Catalyst | Benzyl triethylammonium chloride | HCID 66133 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 58305976 | HCID 58305976 | — |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
356 mg (0.85 mmol) of 2-[1-(cyclopropylmethyl)piperidin-4-yl]-7-(2,4-dichlorophenyl)[1,2,4]-triazolo[1,5-c]pyrimidin-5(6H)-one hydrochloride (Example 46A) were initially charged in phosphorus oxychloride (6 ml), 775 mg (3.40 mmol) of benzyltriethylammonium chloride were added and the mixture was stirred at 120° C. for 2.5 h. The reaction mixture was poured into saturated aqueous sodium bicarbonate solution (150 ml), and solid sodium bicarbonate was added until a pH of 7 had been reached. The mixture was extracted with dichloromethane (3×50 ml), and the combined organic phases were washed with water (50 ml), dried over magnesium sulfate and concentrated. This gave 307 mg (83% of theory) of the product as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436003B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-ddce0dd1f7954abd947554f6720ac734 |
| Source note | uspto-grants-2013_05 |