HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 118390004, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 118389993 | HCID 118389993 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 118390004 | HCID 118390004 | 93.2% |
Reaction Steps
To a solution of tert-butyl 8-((5-methyl-2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)amino)-2-azaspiro[4.5]decane-2-carboxylate (290 mg, 0.66 mmol) in DCM (10 mL) was added a solution of HCl in EtOAc (10 mL, 40 mmol) and the reaction mixture was stirred at rt overnight and then concentrated in vacuo. The residue was dissolved in water (30 mL) and adjusted to pH=10 with a saturated Na2CO3 aqueous solution, then extracted with DCM (100 mL×3). The combined organic phases were washed with brine (100 mL), dried over anhydrous Na2SO4, then filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (MeOH/DCM (v/v)=1/5) to give the title compound as a beige solid (210 mg, 93.2%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403801B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-88a4d69c95b0414eb4fa581b96bc2b14 |
| Source note | uspto-grants-2016_08 |