HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetonitrile → HCID 53312034, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 67320582 | HCID 67320582 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 53312034 | HCID 53312034 | 22.1% |
Reaction Steps
A solution of 100 mg (0.186 mmol) (2-{[4-(2,5-dichloro-phenoxy)-pyridine-3-carbonyl]-methyl-amino}-4,5-difluoro-phenyl)-methyl-carbamic acid tert-butyl ester in 1.5 mL 1M aqueous hydrochloric acid was stirred for 4 hours at 90° C. The reaction mixture was cooled down to room temperature and 2 mL 1M aqueous sodium hydroxide solution and 1 mL acetonitrile were added. The light yellow solution was directly purified by preparative HPLC (Phenomenex Gemini column) with a gradient of acetonitrile:water (containing 0.05% formic acid) (10:90 to 98:2) to give 18 mg (22%) of the title compound as a colorless solid. MS (ESI): m/z=438.058 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08420647B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-2633fe578725430a903a64c0d582942a |
| Source note | uspto-grants-2013_04 |