反应详情

With stirring under nitrogen atmosphere under ice cooling, 80 g of dispiro[4.1.4.3]tetradecan-6-one and 73 g of tetrahydrofuran were added to a mixture of 14.5 g of sodium borohydride, 145 g of methanol, 0.3 g of 25% sodium hydroxide aqueous solution, 8 g of water, and 73 g of tetrahydrofuran. The reaction mixture was stirred overnight at room temperature, and 300 ml of toluene was added thereto, whereupon the organic layer was separated. Through ordinary work-up of extraction, washing and drying, and subsequent concentration under reduced pressure, there was obtained 81.0 g (yield 99%) of the target compound, dispiro[4.1.4.3]-tetradecan-6-ol. This compound had a purity high enough to use in the subsequent step without further purification.

1. stirringThe reaction mixture was stirred overnight at room temperature
2. customwhereupon the organic layer was separated
3. extractionThrough ordinary work-up of extraction
4. washwashing
5. customdrying
6. concentrationsubsequent concentration under reduced pressure