HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 118390008, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 118390054 | HCID 118390054 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 118390008 | HCID 118390008 | 93.1% |
Reaction Steps
To a suspension of tert-butyl 8-((5-chloro-2-((1-methyl-1H-pyrazol-4-yl)amino)pyrimidin-4-yl)(methyl)amino)-2-azaspiro[4.5]decane-2-carboxylate (3.9 B: 0.19 g, 0.40 mmol) in DCM (10 mL) was added a solution of HCl in EtOAc (10 mL, 3.5 M). The mixture was stirred at room temperature for 2 h, then concentrated in vacuo. The residue was diluted with DCM (10 mL) and saturated Na2CO3 aqueous solution (10 mL) and then the mixture was extracted with DCM/MeOH (v/v)=10/1 (30 mL×5). The combined organic layer was dried over anhydrous Na2SO4, then filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/2N NH3 in MeOH (v/v)=5/1) to give 3.10 B as a light yellow solid (0.14 g, 93%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403801B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-f4240c414fdf453c83cd6c18632f3e2f |
| Source note | uspto-grants-2016_08 |