Lithium Hydroxide → HCID 59487505, compound

Temperature

21 °C

To a solution of methyl 2,6-bis(difluoromethyl)benzoate (205 mg) in methanol (3 ml) was added a solution of lithium hydroxide (48 mg) in methanol (3 ml). It was stirred at 21° C. and the initial oily suspension slowly cleared over ca. 2 hours but insoluble material remained. It was stirred for a total of 20 hours and then evaporated to dryness. It was partitioned between ethyl acetate (10 ml) and water (10 ml), washed with ether (10 ml), acidified with 2M hydrochloric acid and extracted with ethyl acetate (2×10 ml). This was washed with water (10 ml) and saturated brine (10 ml), dried over sodium sulphate and evaporated to give the title compound (146 mg).

1. stirringIt was stirred for a total of 20 hours
2. customevaporated to dryness
3. customIt was partitioned between ethyl acetate (10 ml) and water (10 ml)
4. washwashed with ether (10 ml)
5. extractionextracted with ethyl acetate (2×10 ml)
6. washThis was washed with water (10 ml) and saturated brine (10 ml)
7. dry with materialdried over sodium sulphate
8. customevaporated

ORD record

ord-4bc67239047e4c3dbae6ecd7d7ef7f42

Source dataset

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08247377B2