反应详情

Lithium aluminum hydride (80 g) is stirred in ether (2000 ml) while the product of Example 3 (230 g) in ether (250 ml) is added dropwise. When the addition is complete the mixture is stirred an additional 16 hours. The reaction mixture is decomposed by careful addition of water (80 ml) followed by 15% aqueous sodium hydroxide (80 ml) and additional water (240 ml). The resulting suspension is filtered, the filter cake washed with ethanol and ether and the combined filtrates evaporated to give a residue. Distillation of the residue gives the title product (155 g) (81%) B.P. 75° C. (0.05 mm).

1. additionis added dropwise
2. additionWhen the addition
3. filtrationThe resulting suspension is filtered
4. washthe filter cake washed with ethanol and ether
5. customthe combined filtrates evaporated
6. customto give a residue
7. distillationDistillation of the residue