反应详情

A solution of 2-chloro-5-nitro-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide (Example 29a, 0.50 g) and ammonium chloride (0.5 g) were dissolved in 50% aqueous ethanol. Iron powder (0.5 g) was added and the mixture stirred at reflux temperature for 3 h before being cooled and the solids removed by filtration. The mother liquors were treated with 10% sodium hydroxide solution and the product extracted into ethyl acetate. The organic solution was washed with brine, dried over sodium sulphate (Na2SO4) and concentrated to give a residue which was purified by silica gel chromatography to give the sub-title compound as a white solid (0.4 g).

1. temperatureat reflux temperature for 3 h
2. temperaturebefore being cooled
3. customthe solids removed by filtration
4. additionThe mother liquors were treated with 10% sodium hydroxide solution
5. extractionthe product extracted into ethyl acetate
6. washThe organic solution was washed with brine
7. dry with materialdried over sodium sulphate (Na2SO4)
8. concentrationconcentrated
9. customto give a residue which
10. customwas purified by silica gel chromatography