反应详情

8-t-Butyl-1-oxaspiro(4,5)-decane-3-one oxime (17.5 g, 76 mmol) in tetrahydrofuran (50 ml) was added to a solution of lithium- aluminium hydride (4.5 g, 0.125 mol) in tetrahydrofuran (100 ml). The reaction mixture was refluxed for 4 hours, cooled end excess LAH was hydrolysed by addition of saturated aqueous sodium sulfate. solids were filtered off washed with tetrahydrofuran and the solvent was stripped off in vacuo. Kugelrohr distillation of the resulting pale yellow oil (16.9 g) gave a colourless oil (12.3 g) Bp.: 125° C./0.02 mbar, nD22 :1.4840.

1. temperatureThe reaction mixture was refluxed for 4 hours
2. filtrationsolids were filtered off
3. washwashed with tetrahydrofuran
4. distillationKugelrohr distillation of the resulting pale yellow oil (16.9 g)