HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 131736499, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 118390113 | HCID 118390113 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131736499 | HCID 131736499 | 108% |
Reaction Steps
To a solution of tert-butyl 4-((2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)amino)-2-azaspiro[4.4]nonane-2-carboxylate (550 mg, 1.33 mmol) in DCM (20 mL) was added CF3COOH (5 mL) and the reaction mixture was stirred at rt for 2 h. The reaction mixture was concentrated in vacuo and adjust to pH=8˜9 with the saturated NaHCO3 aqueous solution, then diluted with H2O (20 mL) and extracted withed EtOAc (50 mL×3). The combined organic phases were washed with brine (50 mL), then dried over Na2SO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/MeOH (v/v)=50/1 to 10/1) to give the product as a yellow solid (450 mg, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403801B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-19c66575b39e48cca2886f7e38cbe236 |
| Source note | uspto-grants-2016_08 |