HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 6-Chloro-5-fluoropicolinic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 46311229 | HCID 46311229 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 6-Chloro-5-fluoropicolinic acid | HCID 11412672 | 83.5% |
Reaction Steps
Methyl 6-chloro-5-fluoropicolinate (1.35 g, 7.095 mmol) was dissolved in THF:H2O=6:1 (42 ml), followed by addition of lithium hydroxide monohydrate (596 mg, 14.19 mmol), and then the resulting mixture was stirred at room temperature for 3 hours. The resulting reaction liquid was concentrated under reduced pressure, dissolved by addition of distilled water (20 ml), acidified by slow addition of 1N aqueous HCl solution, and then extracted with 5% MeOH/MC (30 ml×2). The organic layer was dried over anhydrous sodium sulfate, followed by filtration, concentration, and vacuum drying, to obtain 1.04 g of white solid (80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096571B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-c5b83226f15349798a0bdb488d92a741 |
| Source note | uspto-grants-2015_08 |