HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 117899599, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 117899603 | HCID 117899603 | — |
| Product | HCID 117899599 | HCID 117899599 | — |
Reaction Steps
Trifluoroacetic acid (1 mL) was added to a solution of tert-butyl 4-{2-[4-(2-cyano-8,9-dimethyl-9H-purin-6-yl)-2-(trifluoromethyl)phenoxy]ethyl}piperidine-1-carboxylate (100 mg) in CH2Cl2 (2 mL)-acetonitrile (0.5 mL) at room temperature, and the mixture was stirred at the same temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, and CH2Cl2 (2 mL) was added to the residue. A 4 M solution of hydrogen chloride in EtOAc (0.2 mL) was added to the mixture at room temperature, and the precipitate was collected by filtration, whereby 8,9-dimethyl-6-{4-[2-(piperidin-4-yl)ethoxy]-3-(trifluoromethyl)phenyl}-9H-purine-2-carbonitrile monohydrochloride (59 mg) was obtained as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09328118B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-2d94a6c13ef44639b4f8ef4546fd16c8 |
| Source note | uspto-grants-2016_05 |