反应详情

温度

0 °C

3.47 g (98 mmol) of lithium aluminium hydride are added to a solution, which is kept at 0° C. and under argon, of 4.95 g (37 mmol) of sublimed anhydrous aluminium chloride and 50 ml of diethyl ether. The resulting complex is stirred at 0° C. for 20 minutes, and then a solution of 11.9 g (37.1 mmol) of the ester obtained in Step D in 130 ml of a mixture of diethyl ether and tetrahydrofuran (10:3) is added rapidly. The whole is kept at 0° C. for 45 minutes. The excess hydride is decomposed by the addition, in succession, of 10 ml of 0.4N hydrochloric acid, 10 ml of 1N hydrochloric acid and 20 ml of 4N hydrochloric acid. After dilution with 100 ml of water, the reaction mixture is extracted with diethyl ether (from 500 to 2000 ml). The ethereal phases are treated in the customary manner, yielding a pale yellow liquid which is used directly in the following step without additional purification.

1. waitThe whole is kept at 0° C. for 45 minutes
2. extractionAfter dilution with 100 ml of water, the reaction mixture is extracted with diethyl ether (from 500 to 2000 ml)
3. additionThe ethereal phases are treated in the customary manner
4. customyielding a pale yellow liquid which
5. customis used directly in the following step without additional purification