HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Methyl 3-(benzyloxy)-4,6-dibromopicolinate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzyl Chloride | HCID 7503 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyl 4,6-dibromo-3-hydroxypicolinate | HCID 22175130 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Methyl 3-(benzyloxy)-4,6-dibromopicolinate | HCID 22175074 | 90.6% |
Reaction Steps
To a stirred mixture of sodium hydride (0.6 g) in DMF (50 mL) was slowly added 14 (7.1 g). After the addition was complete, the mixture was stirred at room temperature for 15 minutes, then benzyl chloride (3.05 g) was added all at once. The mixture was then heated at 90° C. for six hours, cooled, poured into water (500 mL) and extracted with ether (2×200 mL). The ether extracts were combined, washed with 2N NaOH (50 mL), dried (MgSO4) and the solvent was evaporated to give 15 as a light yellow solid (8.3 g). Recrystallization from a small volume of methanol gave an analytical sample, m.p. 75-76° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06706740B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-89ae3bd4012e488db8e1fde26da28f53 |
| Source note | uspto-grants-2004_03 |