Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | [2-(4-Bromo-phenyl)ethyl]-carbamic acid tert-butyl ester | HCID 14221818 | — |
| Catalyst | HCID 178418397 | HCID 178418397 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 71150146 | HCID 71150146 | 117.1% |
Reaction Steps
IMS (600 mL) and water (250 mL) were degassed thoroughly. tert-Butyl 4-bromophenethylcarbamate (32.7 g, 109 mmol), sodium carbonate (46.2 g, 436 mmol), palladium tetrakis (12.6 g, 11.0 mmol) and 2-methoxypyridine boronoic acid (25.0 g, 163 mmol) were added and the reaction mixture heated to 90° C. for 18 hours. The reaction was cooled to room temperature, filtered and the residue washed with IMS (100 mL) and ethyl acetate (1 L). The filtrate was washed with water (500 mL), dried (MgSO4) and concentrated to give a brown solid. The crude residue was subject to column chromatography (0 to 1.5% MeOH in DCM) to give a white solid, tert-butyl 4-(6-oxo-1,6-dihydropyridin-3-yl)phenethylcarbamate (20.95 g, 63.8 mmol, 58% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09415045B2 |
|---|
| Source dataset | uspto-grants-2016_08 |
|---|
| ORD ID | ord-155152fc6d9d4d078c3294344c8c8e7b |
|---|
| Source note | uspto-grants-2016_08 |
|---|