HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 118390106, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | HCID 118390028 | HCID 118390028 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 118390106 | HCID 118390106 | 48.5% |
Reaction Steps
To a solution of tert-butyl 4-((5-methyl-2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)amino)-2-azaspiro[4.4]nonane-2-carboxylate (0.35 g, 0.82 mmol) in DCM (10 mL) was added a solution of HCl in EtOAc (2.83 M, 5 mL) and the reaction mixture was stirred at rt for 16 h then added water (10 mL). The resulting mixture was adjusted to pH=8 with a saturated Na2CO3 aqueous solution, then extracted with DCM (20 mL×3). The combined organic layers were washed with brine dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=10/1) to give the product as a yellow solid (0.13 g, 48.5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403801B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-f07bdd4cbaf34dd0836d6bd776070e32 |
| Source note | uspto-grants-2016_08 |