HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 67981041, compound → HCID 68048119, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 67981041 | HCID 67981041 | — |
| Solvent | Acetic Acid Mixture with Hydrobromic Acid | HCID 21893785 | — |
| Product | HCID 68048119 | HCID 68048119 | 66% |
Reaction Steps
A solution of benzyl 5-(2-methylpyrimidin-4-ylcarbamoyl)bicyclo[3.2.1]octan-1-ylcarbamate (1 g, 2.5 mmol) in HBr/HOAc (33% solution, 8 mL) was stirred at room temperature for an hour and then concentrated under reduced pressure. The resulting residue was dissolved in aq. HCl (6N, 10 mL) and extracted with ethyl acetate (10 mL) to remove the organic impurities. The aqueous phase was basified with aq. NaOH (6N, 4 mL), and then extracted with DCM (4×20 mL). The combined organic layer was washed with brine, dried over Na2SO4 and concentrated under reduced pressure to afford 350 mg (66%) of 5-amino-N-(2-methylpyrimidin-4-yl)bicyclo[3.2.1]octane-1-carboxamide as a white solid ESI-MS m/z: 261 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08921370B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-7602d63dec5547feb9b864df9dfd426c |
| Source note | uspto-grants-2014_12 |