反应详情

Dissolve in 9.0 g of the title compound of Example 28 in 80 ml of tetrahydrofuran. Add the resulting solution (drop by drop over a period of 10 minutes while stirring at 0°) to a suspension of 1.30 g of lithium aluminum hydride (=lithium hydridoaluminate) in 30 ml of tetrahydrofuran. Then boil the prepared admixture for 1.5 hours under reflux before adding a further 2.0 g of lithium aluminum hydride thereto and boiling for a further 3.5 hours under reflux. Cool the refluxed product to ambient temperature. Carefully add 300 ml of water to the cooled material and extract it 3 times with 50 ml of diethyl ether (each time). Wash the combined ether solutions with saturated common salt solution. Dry the washed solutions over sodium sulfate. Evaporate off the solvent in vacuo. Distil the residue to obtain 5.89 g of the title compound with a BP at 115° at 0.01 mm of Hg.

1. additionAdd the resulting solution (drop by drop over a period of 10 minutes
2. customfor 1.5 hours
3. temperatureunder reflux
4. temperatureunder reflux
5. extractionCarefully add 300 ml of water to the cooled material and extract it 3 times with 50 ml of diethyl ether (each time)
6. washWash the combined ether solutions with saturated common salt solution
7. dry with materialDry the washed solutions over sodium sulfate
8. customEvaporate off the solvent in vacuo
9. customDistil the residue