HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86703127, compound → HCID 86703126, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86703127 | HCID 86703127 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86703126 | HCID 86703126 | — |
Reaction Steps
A mixture of 5-azido-1,3-dimethyl-tetrahydro-pyrimidin-2-one (Step P5) (2.5 g, 11.1 mmol) and Pd/C 10% (500 mg) in EtOH (70 mL) was stirred at rt under a hydrogen atmosphere for 13.5 h. The reaction mixture was filtered through a pad of celite, washed with THF and MeOH and concentrated. The residue was dissolved in EtOAc and extracted with cold 1N HCl. The aqueous phase was basified with a saturated aqueous NaHCO3 solution. The resulting aqueous phase was extracted with CH2Cl2/isopropanol 3:1 (3×). The combined organic layers were dried (Na2SO4), filtered and concentrated to afford the title compound. ESI-MS: [M+H]+ 144.1 (MS 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09365576B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-6da39042df724714b7d1c5a0d66477ee |
| Source note | uspto-grants-2016_06 |