反应详情

To the mixture of 486 mg of lithium aluminum hydride (12.3 mmol) and 20 ml of diethylether in a 100 ml two-neck flask, 20 ml of a diethylether solution containing 643 mg of tricyclohexyl[o-(1-azidoethyl)phenyl]tin (1.25 mmol) was added dropwise, followed by a heat-refluxing for 11.5 hours. Upon completion of the reaction, the organic layer was separated using 10 ml of water. After the ether layer was washed with 30 ml of a saturated brine and dried over sodium sulfate, the solvent was removed under reduced pressure to yield a crude product. The resultant crude product was purified by column chromatography on silica gel (for which, 25 g of silica gel, and hexane as a development solvent were employed) to yield 467 mg of the final product (yield=76.5%).

1. additionwas added dropwise
2. customheat-refluxing for 11.5 hours
3. customUpon completion of the reaction
4. customthe organic layer was separated
5. washAfter the ether layer was washed with 30 ml of a saturated brine
6. dry with materialdried over sodium sulfate
7. customthe solvent was removed under reduced pressure
8. customto yield a crude product
9. customThe resultant crude product was purified by column chromatography on silica gel (for which, 25 g of silica gel, and hexane as a development solvent