反应详情

温度

-78 °C

Under the argon atmosphere, the compound (165 mg) produced in Example 100 was dissolved in DME (2 mL), the solution was cooled to −78° C., followed by addition of a 0.5M potassium hexamethyldisilazane/toluene solution (0.90 mL). After stirring the mixture at −78° C. for 20 minutes, a DME (1.5 mL) solution of the compound produced in Example 13 was added dropwise, and stirring at the same temperature was carried out for 10 minutes. After raising a temperature of the reaction solution to 0° C., water was added, and the extract obtained by extraction with ethyl acetate was washed with water and a saturated saline; dried with anhydrous magnesium sulfate; and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:10→65:35) to obtain a titled compound (177 mg) having the following physical property values.

1. stirringstirring at the same temperature
2. waitwas carried out for 10 minutes
3. temperatureAfter raising a temperature of the reaction solution to 0° C.
4. washwas washed with water
5. dry with materialdried with anhydrous magnesium sulfate
6. concentrationand concentrated under reduced pressure
7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:10→65:35)