Hydrochloric Acid → HCID 56706473, compound

Temperature

80 °C

Under a nitrogen atmosphere at 0° C., to a solution (4 mL) of the compound (7.4 g, 25 mmol) obtained in Example 64a in tetrahydrofuran was added lithium tetrahydroborate (2.6 g, 49 mmol), and the mixture was stirred at 80° C. for 5 hr. 1N Hydrochloric acid was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The resulting crude title compound was purified by column chromatography (hexane-hexane/ethyl acetate=50/50) to give the title compound (5.4 g, 85%) as a colorless solid.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe obtained organic layer was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. customThe solvent was evaporated under reduced pressure
5. customThe resulting crude title compound was purified by column chromatography (hexane-hexane/ethyl acetate=50/50)

ORD record

ord-a4e367100d824ce5a197745f14e5ce56

Source dataset

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08461348B2