反应详情

In 10 ml of methylene chloride was dissolved 0.50 g of 1α,3β-dihydroxypregna-5,7-diene-20-carbaldehyde, followed by addition of 1 ml of 3,4-dihydropyran and 0.05 g of p-toluenesulfonic acid. The mixture was stirred at room temperature for 2 hours. The reaction mixture thus obtained was diluted with ether, washed successively with aqueous sodium hydrogen carbonate solution and aqueous sodium chloride solution, and dried over sodium sulfate, followed by concentration under reduced pressure. Finally the concentrate was purified by column chromatography to give 0.48 g of 1α,3β-bis(tetrahydropyran-2-yloxy)pregna-5,7-diene-20-carbaldehyde showing the following physical properties.

1. customThe reaction mixture thus obtained
2. washwashed successively with aqueous sodium hydrogen carbonate solution and aqueous sodium chloride solution
3. dry with materialdried over sodium sulfate
4. concentrationfollowed by concentration under reduced pressure
5. customFinally the concentrate was purified by column chromatography