反应详情

To a suspension of lithium aluminum hydride (12 g, 0.32 mol, 2.25 equivalents) in refluxing THF (150 mL), under a nitrogen atmosphere, was added, dropwise over a period of 30 minutes, a solution of 1-cyano-1-trimethylsilyloxy-1,2,3,4-tetrahydronaphthalene, from Step 1, in 150 mL of THF. The resulting mixture was refluxed for 4 hours and then cooled to ambient temperature and diluted with THF. Sodium sulfate decahydrate was added to quench the excess lithium aluminum hydride. The solids were filtered over Celite® filter aid. The filtrate was then concentrated to give a light brown, waxy solid which was used in the next step without purification.

1. additionunder a nitrogen atmosphere, was added, dropwise over a period of 30 minutes
2. temperatureThe resulting mixture was refluxed for 4 hours
3. customto quench the excess lithium aluminum hydride
4. filtrationThe solids were filtered over Celite®
5. filtrationfilter aid
6. concentrationThe filtrate was then concentrated
7. customto give a light brown, waxy solid which
8. customwas used in the next step without purification