反应详情

温度

100 °C

2-Amino-4-(4-nitrophenoxy)pyridine (300 mg), 4-chlorobutyryl chloride (0.18 ml), triethylamine (0.77 ml), dimethylformamide (1 ml) and tetrahydrofuran (1 ml) were stirred at room temperature for 10 minutes, and then silica gel was added to the reaction solution, the solvent was distilled off under reduced pressure and the reaction product was adsorbed onto the silica gel. The silica gel was charged into a dry column packed with silica gel, for column purification (hexane:ethyl acetate=3:1, followed by 2:1 and 1:1). The solvent was distilled off under reduced pressure, and then 300 mg of iron powder, 600 mg of ammonium chloride, 2 ml of DMF, 1 ml of ethanol and 1 ml of water were added to 150 mg of the resulting residue and the mixture was stirred at 100° C. for 20 minutes. After filtration with celite, water and ethyl acetate were added for extraction. The organic layer was washed 5 times with ammonium chloride water and then dried over magnesium sulfate. The drying agent was filtered off and the solvent was distilled off under reduced pressure to obtain 110 mg of the target substance as an oil.

1. additionsilica gel was added to the reaction solution
2. distillationthe solvent was distilled off under reduced pressure
3. additionThe silica gel was charged into a dry column
4. custompacked with silica gel, for column purification (hexane:ethyl acetate=3:1, followed by 2:1 and 1:1)
5. distillationThe solvent was distilled off under reduced pressure
6. addition300 mg of iron powder, 600 mg of ammonium chloride, 2 ml of DMF, 1 ml of ethanol and 1 ml of water were added to 150 mg of the resulting residue
7. filtrationAfter filtration with celite, water and ethyl acetate
8. additionwere added for extraction
9. washThe organic layer was washed 5 times with ammonium chloride water
10. dry with materialdried over magnesium sulfate
11. filtrationThe drying agent was filtered off
12. distillationthe solvent was distilled off under reduced pressure
13. customto obtain 110 mg of the target substance as an oil