反应详情

温度

23 °C

To a mixture of 82.27 g sodium hydride (80%) in 2.1 L tetrahydrofuran was slowly added the solution of 208 g (1.03 mol) 8-(methoxymethyl)-1,4-dioxaspiro[4.5]decan-8-ol (prepared according to intermediate example 16f) in 1 L tetrahydrofuran under cooling. After 0.5 hours at 23° C. 143 mL iodomethane were added and the mixture was stirred at 23° C. overnight. Water was added and the mixture was extracted with ethyl acetate. The combined organic layers were washed with brine and dried over sodium sulfate. After filtration and removal of the solvent 227.5 g (max. 100%) of the title compound were obtained that was used without further purification.

1. temperatureunder cooling
2. extractionthe mixture was extracted with ethyl acetate
3. washThe combined organic layers were washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationAfter filtration and removal of the solvent 227.5 g (max. 100%) of the title compound
6. customwere obtained
7. customthat was used without further purification