反应详情

29.2 g of the product from (i) in 200 ml of acetic acid was added to 300 ml of 6 M hydrochloric acid to give a fine precipitate. To this was assed a zinc amalgam (made by intimately mixing 60 g of zinc, 6 g of mercury (II) chloride, 5 ml of conc. hydrochloric acid and 90 ml of water over 20 minutes. The mixture was heated at reflux for 5 hours; three further portions of 60 ml of conc. hydrochloric acid being added. After cooling, the filtered solids were taken up in chloroform, refiltered, and washed with 6 M hydrochloric acid, then water, dried and evaporated to give 26 g of the crude product. This was recrystallised from light petroleum (b.p. 60°-80° C.) to give 22.9 g of the product with a melting point of from 81°-82.5° C.

1. customto give a fine precipitate
2. temperatureThe mixture was heated
3. temperatureat reflux for 5 hours
4. temperatureAfter cooling
5. washwashed with 6 M hydrochloric acid
6. dry with materialwater, dried
7. customevaporated
8. customto give 26 g of the crude product
9. customThis was recrystallised from light petroleum (b.p. 60°-80° C.)