Hydrochloric Acid → HCID 58288276, compound

Temperature

40 °C

3.77 g (crude, about 11.5 mmol) of ethyl (3R)-2-(3,4-dichlorophenyl)-4,4,4-trifluoro-3-methylbutanoate (diastereomer mixture) were dissolved in a mixture of 14 ml of methanol, 14 ml of THF and 5 ml of water, and 9.16 g of 50% strength aqueous sodium hydroxide solution were added at 0° C. The reaction mixture was stirred at 40° C. for about 6 h. The mixture was then acidified with 1 N hydrochloric acid (pH about 2) and extracted three times with ethyl acetate. The combined organic phases were washed with sat. sodium chloride solution, dried over sodium sulphate and concentrated under reduced pressure. This gave 3.94 g of the target compound as a crude product which could be used without further purification for subsequent reactions.

1. additionwere added at 0° C
2. extractionextracted three times with ethyl acetate
3. washThe combined organic phases were washed with sat. sodium chloride solution
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated under reduced pressure
6. customThis gave 3.94 g of the target compound as a crude product which could be used without further purification for subsequent reactions

ORD record

ord-497d6b534d154036aba30bc369b02dd6

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09018414B2