反应详情

A solution of 2-(4-dimethoxymethyl-2-methoxy-3-nitrophenoxy)ethylamine (0.5 g, 1.8 mmol) obtained in Step 3 in THF (10 mL) was added with triethylamine (0.38 mL, 2.7 mmol) and n-propanesulfonyl chloride (0.24 mL, 2.2 mmol), followed by stirring at room temperature for 3 hours. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure. The residue was added with methanol (6.0 mL) and 1 mol/L hydrochloric acid, followed by stirring for 15 minutes. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure to obtain [2-(4-formyl-2-methoxy-3-nitrophenoxy)ethyl]propane-1-sulfonamide (0.39 g, 62%).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was evaporated under reduced pressure
5. additionThe residue was added with methanol (6.0 mL) and 1 mol/L hydrochloric acid
6. stirringby stirring for 15 minutes
7. additionThe reaction mixture was added with water
8. extractionextracted with ethyl acetate
9. washThe organic layer was washed with saturated brine
10. dry with materialdried over anhydrous magnesium sulfate
11. customthe solvent was evaporated under reduced pressure