HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 89544968, compound → HCID 89544821, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 89544968 | HCID 89544968 | — |
| Catalyst | HCID 178418406 | HCID 178418406 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 89544821 | HCID 89544821 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
Step 3 A stirred suspension of {6-chloro-2-fluoro-3-[(1R)-1-(methylamino)propyl]-phenyl}(pyridin-3-yl)methanol (0.123 g, 0.398 mmol) and manganese(IV) oxide (0.693 g, 7.97 mmol) in toluene (1.99 mL) and 1,2-dichloroethane (1.99 mL) was heated at 100° C. for 2.5 hours. Upon cooling, the mixture was filtered; the residual solids were washed with DCM (×2) and concentrated. Preparative HPLC gave [(1R)-1-{4-chloro-2-fluoro-3-[(pyridin-3-yl)carbonyl]phenyl}propyl](methyl)amine which was converted to the HCl salt, 0.012 g, 9%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145354B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-df9713624c984f118dc5b63215350078 |
| Source note | uspto-grants-2015_09 |