反应详情

A solution of tert-butyl-2-carboxy-3-tert-butoxy-5-thiophenecarboxylate (3 g, 0.01 mmol) in dry acetone (100 ml) was treated, at 0° C., with triethylamine (1.7 ml, 0.012 mmol) added dropwise. The mixture was stirred for 15 minutes and ethyl chloroformate (1.25 ml, 0.013 mmol) added dropwise, at 0° C. After 30 minutes, sodium azide (1.1 g, 0.017 mmol) in water (5 ml) was slowly added, at 0° C. After 4 hours, stirring at ambient temperature, the reaction mixture was filtered and the solvent evaporated. The oily residue was dissolved in CH2Cl2, and the solution washed (2×) with water, dried over MgSO4 and the solvent evaporated to give title compound (3.25 g, 100%).

1. additionadded dropwise
2. waitAfter 30 minutes
3. waitAfter 4 hours
4. stirringstirring at ambient temperature
5. filtrationthe reaction mixture was filtered
6. customthe solvent evaporated
7. dissolutionThe oily residue was dissolved in CH2Cl2
8. washthe solution washed (2×) with water
9. dry with materialdried over MgSO4
10. customthe solvent evaporated