反应详情

A stirred mixture of N-(5-cyclopropyl-2-nitrophenyl)-1-(tetrahydro-2H-pyran-4-yl)-4-piperidinamine (D44, 150 mg, 0.43 mmol) and tin (II) chloride (326 mg, 1.72 mmol) in ethanol (10 ml) was treated with conc. HCl acid (˜0.38 ml) and heated at reflux temperature with stirring for 18 hrs. The solvent was removed by concentration under vacuum and the residue treated with dilute K2CO3 solution and extracted with ethyl acetate, filtering the mixture to remove tin residues. The separated organic phase was washed with water and brine, dried (MgSO4) and concentrated under vacuum to afford the title compound as a very pale brown sticky gum (114 mg, 83%). M++H=316.1.

1. temperatureheated
2. temperatureat reflux temperature
3. customThe solvent was removed by concentration under vacuum
4. additionthe residue treated with dilute K2CO3 solution
5. extractionextracted with ethyl acetate
6. filtrationfiltering the mixture
7. customto remove tin residues
8. washThe separated organic phase was washed with water and brine
9. dry with materialdried (MgSO4)
10. concentrationconcentrated under vacuum