反应详情

With stirring under nitrogen atmosphere at room temperature, a mixture of 13.4 g of 8-spiro[4.5]decanone and 80 ml of tetrahydrofuran was added dropwise to a tetrahydrofuran solution of 0.205 mol methylmagnesium chloride (which had been prepared from 5.0 g of metallic magnesium, 100 ml of tetrahydrofuran and chloromethane), during which time the temperature was kept below 50° C. The reaction mixture was cooled to room temperature, after which a saturated ammonium chloride aqueous solution was added to stop the reaction. Through ordinary work-up of extraction, washing and drying, and subsequent concentration under reduced pressure, there was obtained 14.43 g (yield 99%) of the target compound, 8-methylspiro[4.5]decan-8-ol. This compound had a purity high enough to use in the subsequent step without further purification.

1. customwas kept below 50° C
2. temperatureThe reaction mixture was cooled to room temperature
3. customthe reaction
4. extractionThrough ordinary work-up of extraction
5. washwashing
6. customdrying
7. concentrationsubsequent concentration under reduced pressure