HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → 960249-94-9
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Methyl 2-(difluoromethoxy)-6-fluorobenzoate | HCID 59487507 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 960249-94-9 | HCID 46311647 | 60.9% |
Reaction Steps
To a solution of methyl 2-[(difluoromethyl)oxy]-6-fluorobenzoate (800 mg) in anhydrous dioxane (20 ml) was added a solution of lithium hydroxide (260 mg) in water (10 ml). It was stirred for 15 hours, evaporated, dissolved in water (25 ml) and extracted with ethyl acetate (25 ml) and ether (25 ml). The aqueous phase was acidified with 5M hydrochloric acid and extracted with ethyl acetate (2×25 ml). The combined organic phases were washed with water (10 ml) and saturated brine (10 ml), dried over Na2SO4 and evaporated to give an oil which crystallised (616.3 mg). It was triturated with heptane (ca. 10 ml) and filtered off to give the title compound (456 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247377B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-0cf77176b0b042bc981ba51d11c8b308 |
| Source note | uspto-grants-2012_08 |