Water → HCID 18346021、化合物

温度

0 °C

To a solution of (S)-Hexahydro-[1,2,3]oxathiazolo[3,4-a]pyridine 1-oxide (1.31 g, 8.125 mmol) in anhydrous acetonitrile (10 mL) was added sodium (meta)periodate (1.91 g, 8.9375 mmol), followed by ruthenium(III) chloride hydrate (17 mg, 0.08125 mmol), and then H2O (10 mL). The mixture was stirred at 0° C. for 10 min and at rt for 20 min, then diluted with saturated NaHCO3 (30 mL) and EtOAc (100 mL). The aqueous layer was extracted with EtOAc (80 mL) and DCM (80 mL). The combined organic layer was dried over Na2SO4, concentrated in vacuo, and purified by flash column chromatography (silica gel, 2% EtOAc in DCM) to afforded the title product as a clear, colorless oil (1.1 g, 76%).

1. extractionThe aqueous layer was extracted with EtOAc (80 mL) and DCM (80 mL)
2. dry with materialThe combined organic layer was dried over Na2SO4
3. concentrationconcentrated in vacuo
4. custompurified by flash column chromatography (silica gel, 2% EtOAc in DCM)

ORDレコード

ord-0d765edc1a0e457fab266ae815921fb6

出典データセット

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08598359B2