反应详情

A solution of 1.1 g (4.5 mmol) of the compound of Step 1 in 10 mL of THF is poured dropwise into 0.21 g (5.4 mmol) lithium aluminium hydride suspended in 5 mL of THF, at ambient temperature, and is then stirred at ambient temperature for 5 hours. Cooling to about 0° C. is carried out and there are then added, cautiously, in succession, 0.14 mL of water, 0.11 mL of 20% aqueous sodium hydroxide solution and 0.51 mL of water. Stirring is carried out overnight at ambient temperature, and then the salts are filtered off over a frit and rinsed with THF. The combined filtrates are concentrated to yield the desired product.

1. temperatureCooling to about 0° C.
2. additionthere are then added
3. stirringStirring
4. waitis carried out overnight at ambient temperature
5. filtrationthe salts are filtered off over a frit
6. washrinsed with THF
7. concentrationThe combined filtrates are concentrated