HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 59418698, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Methoxybenzyl bromide | HCID 165021 | — |
| Reactant | Methyl 6-bromo-3-hydroxypicolinate | HCID 22175135 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 59418698 | HCID 59418698 | — |
Reaction Steps
4-Methoxybenzyl bromide (0.095 g, 0.47 mmol) was added dropwise to a suspension of methyl 6-bromo-3-hydroxypicolinate (26B) (0.100 g, 0.43 mmol) and K2CO3 (0.089 g, 0.65 mmol) in anhydrous acetone (2.5 mL). The reaction mixture was heated at reflux for 3.5 hours, cooled to rt, and concentrated under reduced pressure. Water was added and the mixture extracted with DCM. The organic phases were washed with 1 M NaOH, brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The concentrate was purified by column chromatography on silica gel eluting with a gradient of PE:EtOAc 84:16 to 72:28, to provide the desired product methyl 6-bromo-3-(4-methoxybenzyloxy)picolinate (40A).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067928B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-5f73d23ae62b40a2a126710280993e7e |
| Source note | uspto-grants-2015_06 |