HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → Methyl 6-bromo-3-hydroxypicolinate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Methyl 3-Hydroxy-2-pyridinecarboxylate | HCID 819341 | — |
| Solvent | Water | HCID 962 | — |
| Product | Methyl 6-bromo-3-hydroxypicolinate | HCID 22175135 | 70.7% |
Reaction Steps
To a mechanically stirred solution of methyl 3-hydroxypicolinate (30.6 g) in water (800 mL) was slowly added bromine (32 g) over a 30 minute period. After the addition was complete, stirring was continued for an additional hour. Ether (300 mL) was added and stirring continued until all the solids had dissolved. The organic layer was separated and the aqueous phase extracted with ether (200 mL). The organic phases were combined, dried (MgSO4) and the solvent evaporated to give 32.8 g of methyl 6-bromo-3-hydroxypicolinate as an off-white solid. Recrystallization from methanol/water gave an analytical sample, m.p. 115-117° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06706740B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-409760df93f049d191399ae263fb4d8d |
| Source note | uspto-grants-2004_03 |