HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 118390053, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 118390058 | HCID 118390058 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 118390053 | HCID 118390053 | 97.1% |
Reaction Steps
To a solution of tert-butyl 4-((5-chloro-2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)amino)-2-azaspiro[4.4]nonane-2-carboxylate (650 mg, 1.45 mmol) in DCM (20 mL) was added CF3COOH (5 mL) and the reaction mixture was stirred at rt for 2 hours. The reaction mixture was concentrated in vacuo and adjusted to pH=8-9 with a saturated Na2CO3 solution, then the mixture was diluted with H2O (20 mL) and extracted with 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)=10/1 to 5/1) to give the product as a white solid (490 mg, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403801B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-c5ed30de28664e58bf98b41dd042bc2b |
| Source note | uspto-grants-2016_08 |