Lithium Hydroxide → HCID 18670371, compound

Temperature

45 °C

To a solution of ester 203 (8.06 g, 31.1 mmol) in THF (100 mL) was added an aqueous solution of LiOH (1.96 g, 46.6 mmol) in water (30 mL) and the reaction mixture was allowed to stir at 45° C. for 60 min. Then more LiOH (0.5 g, 11.9 mmol) was added to the heating solution. After further heating for 8 h, the reaction mixture was concentrated, extracted with AcOEt. The extract was concentrated and the residue was combined with the white solid which was collected by filtration from the aqueous phase. The combined solid materials were dissolved in DCM, treated with 2N HCl in diethyl ether (10 mL) and the mixture was diluted with benzene, evaporated and dried under vacuum to give (presumably) mono-hydrochloride salt of the acid 204 (8.23 g, 99% yield).

1. temperatureAfter further heating for 8 h
2. concentrationthe reaction mixture was concentrated
3. extractionextracted with AcOEt
4. concentrationThe extract was concentrated
5. filtrationwas collected by filtration from the aqueous phase
6. dissolutionThe combined solid materials were dissolved in DCM
7. additiontreated with 2N HCl in diethyl ether (10 mL)
8. additionthe mixture was diluted with benzene
9. customevaporated
10. customdried under vacuum

ORD record

ord-b5fe92970215406e95ed19bfb8b24a86

Source dataset

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08598168B2