反应详情

In a 1-liter flask there was placed 19 g of the perchlorate of step (c) above, 300 cc of 95% ethanol and 40 g of zinc powder. There was added from a flask 100 ml of concentrated hydrochloric acid. Mild reflux could be observed during the addition of the acid. The mixture was allowed to stand at room temperature for 10 hours. It was then concentrated, washed with water and extracted with methylene chloride. It was made alkaline with sodium hydroxide and filtered through Celite (Trade Mark). After decanting, drying and evaporating the solvents there were obtained 6 g of a product, insoluble in ether, melting at 250° C. The results of analysis are as follows:

1. customIn a 1-liter flask there was placed
2. temperatureMild reflux could
3. additionbe observed during the addition of the acid
4. concentrationIt was then concentrated
5. washwashed with water
6. extractionextracted with methylene chloride
7. filtrationfiltered through Celite (Trade Mark)
8. customAfter decanting
9. customdrying
10. customevaporating the solvents