反应详情

To a solution of 6.5 g (0.023 m) of 1-[(2-nitrophenyl)methyl]-1-(4-chlorophenyl)hydrazine of Example 12a in 150 ml of 95% ethanol and 25 ml of water, 12.8 g (0.23 g-atom) of iron and 1 ml of concentrated HCl was added. The mixture was refluxed for 0.5 hours, cooled, Celite added and filtered. The filtrate was evaporated and the residual material was partitioned between 10% NaOH and ether. The ether extract was dried (Na2SO4), filtered and evaporated to afford a solid which was triturated with hexane and filtered giving 4.5 g (80%) of 1-[(2-aminophenyl)methyl]-1-(4-chlorophenyl)hydrazine, m.p. 83°-87° C.

1. temperatureThe mixture was refluxed for 0.5 hours
2. temperaturecooled
3. additionCelite added
4. filtrationfiltered
5. customThe filtrate was evaporated
6. customthe residual material was partitioned between 10% NaOH and ether
7. extractionThe ether extract
8. dry with materialwas dried (Na2SO4)
9. filtrationfiltered
10. customevaporated
11. customto afford a solid which
12. customwas triturated with hexane
13. filtrationfiltered