反应详情

To a methanol solution (2.3 mL) of the compound (180 mg) produced in Example 13, potassium carbonate (94 mg) and a Bestmann reagent (dimethyl-1-diazo-2-oxopropyl phosphonate) (105 mg) were added, followed by stirring at room temperature for 6 hours. Further, potassium carbonate (47 mg) and the Bestmann reagent (53 mg) were added, followed by stirring at room temperature overnight. The reaction mixture was cooled to 0° C.; diluted with ethyl acetate; and then separated by adding water. The organic layer was washed with water and a saturated saline; dried with magnesium sulfate; then filtered; and concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=97:3→65:35) to obtain a titled compound (47 mg) having the following physical property values.

1. stirringby stirring at room temperature overnight
2. temperatureThe reaction mixture was cooled to 0° C.
3. customand then separated
4. additionby adding water
5. washThe organic layer was washed with water
6. dry with materialdried with magnesium sulfate
7. filtrationthen filtered
8. concentrationand concentrated under reduced pressure
9. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=97:3→65:35)