HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 24986454, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-Methyl-1h-1,2,3-benzotriazole-5-carbonyl chloride | HCID 2776550 | — |
| Reactant | HCID 67265741 | HCID 67265741 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 24986454 | HCID 24986454 | 48.6% |
Reaction Steps
To a solution of 0.050 g (0.21 mmol) of (+/−)9-amino-2-pyridin -4-yl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one dissolved in 2.2 mL of tetrahydrofuran was added 30 μl (0.25 mmol) of triethylamine and 0.0484 g (0.25 mmol) of 1-methyl-1H-1,2,3-benzotriazole-5-carbonyl chloride. The resulting mixture was stirred at room temperature for 16 h. Water was added and the mixture extracted with ethyl acetate. The extracts were washed with a saturated aqueous solution of ammonium chloride, dried and evaporated. The residue was purified by silica gel chromatography, eluting with dichloromethane/methanol/ammonia in the proportions 95/5/0.5 to give 0.041 g of pure product obtained in the form of free base.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08198287B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-2ac0c5045780416abe07a20d3cea8703 |
| Source note | uspto-grants-2012_06 |