Tetrahydrofuran → HCID 66962053, compound

A solution of 3.23 g (13.91 mmol) of the title compound in step (i) of Example XA1 in tetrahydrofuran (31.3 ml) was cooled to 0° C. Lithiumaluminum hydride (2.11 g, 55.62 mmol) was then added thereto, and the mixture was stirred for 2.5 hr. Thereafter, the reaction solution was stirred at room temperature for one hr. Lithium aluminum hydride (0.528 g, 13.91 mmol) was added thereto, and the mixture was stirred at room temperature for one hr. A saturated aqueous sodium potassium tartrate solution was added thereto, and the mixture was extracted with diethyl ether. The extract was dried over anhydrous sodium sulfate and was then filtered. The filtrate was concentrated at a low temperature under the reduced pressure. The residue was purified by column chromatography on silica gel (hexane:diethyl ether=1:1 to 1:4) to give the title compound as a crude product.

1. customwas cooled to 0° C
2. stirringThereafter, the reaction solution was stirred at room temperature for one hr
3. stirringthe mixture was stirred at room temperature for one hr
4. extractionthe mixture was extracted with diethyl ether
5. dry with materialThe extract was dried over anhydrous sodium sulfate
6. filtrationwas then filtered
7. concentrationThe filtrate was concentrated at a low temperature under the reduced pressure
8. customThe residue was purified by column chromatography on silica gel (hexane:diethyl ether=1:1 to 1:4)

ORD record

ord-63ea9fdfd29d4dcaaa90be97410ce27a

Source dataset

uspto-grants-2011_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07879808B2