反应详情

4-(4-Chloro-phenoxymethyl)-benzylazide (3.2 g, 11.7 mmol) was dissolved in MeOH (50 mL). NEt3 (11.35 mL, 81.9 mmol) and SnCl2×2H2O (5.28 g, 23.4 mmol) were added and the exothermic reaction was stirred under reflux. When boiling ceased the mixture was heated to reflux for additional 45 min. After cooling to r.t. the mixture was filtered and the filtrate was evaporated to dryness. The residue was dissolved in CH2Cl2 (300 mL) and this solution was washed with sat. aq. NaHCO3-solution (1×100 mL), dried over Na2SO4, filtered and evaporated to dryness to give the title compound, pure enough for further reaction.

1. customthe exothermic reaction
2. temperatureunder reflux
3. temperaturewas heated
4. temperatureto reflux for additional 45 min
5. filtrationwas filtered
6. customthe filtrate was evaporated to dryness
7. dissolutionThe residue was dissolved in CH2Cl2 (300 mL)
8. washthis solution was washed with sat. aq. NaHCO3-solution (1×100 mL)
9. dry with materialdried over Na2SO4
10. filtrationfiltered
11. customevaporated to dryness