反应详情

A solution of the isourea from Step 1. above (208.9 g) in anhydrous THF (500 ml) is added dropwise to a stirred suspension of 60% sodium hydride dispersion (57.0 g) in anhydrous THF (750 ml) and the reaction mixture is refluxed for 2 hours. Distilled water (450 ml) is added dropwise to the stirred mixture which is washed with diethyl ether. 20% sulfuric acid (400 ml) is added slowly to the stirred reaction mixture, which is extracted with methylene chloride, dried, filtered, and the filtrate evaporated and dried under high vacuum yielding the desired product as a crude solid which is used in the next step without further purification.

1. temperaturethe reaction mixture is refluxed for 2 hours
2. washis washed with diethyl ether
3. addition20% sulfuric acid (400 ml) is added slowly to the stirred reaction mixture, which
4. extractionis extracted with methylene chloride
5. customdried
6. filtrationfiltered
7. customthe filtrate evaporated
8. customdried under high vacuum