反应详情

温度

0 °C

Dissolve 7-methyl-1,4-dioxa-spiro[4.5]decan-8-one (11.45 g, 67.28 mmol) in THF (300 mL) and cool the solution to 0° C. under N2. Add super-hydride (74.0 mL, 74.0 mmol, 1 M in THF) and stir the reaction mixture overnight. Add water (200 mL), and extract the aqueous layer with dichloromethane (3×300 mL). Combine the organic layers and dry with Na2SO4, filter, concentrate and purify by flash column chromatography (silica gel, 30-50% of EtOAc/Hexane) to give cis-7-Methyl-1,4-dioxa-spiro[4.5]decan-8-ol.

1. extractionAdd water (200 mL), and extract the aqueous layer with dichloromethane (3×300 mL)
2. dry with materialCombine the organic layers and dry with Na2SO4
3. filtrationfilter
4. concentrationconcentrate
5. custompurify by flash column chromatography (silica gel, 30-50% of EtOAc/Hexane)