反应详情

温度

100 °C

3-Aminophenol (0.050 mol) was dissolved in DMA (100 mL). K2CO3 (0.060 mol) was added. 4-Chloro-2-dimethoxymethyl-1-nitrobenzene (0.050 mol) was added, and the reaction mixture was stirred overnight at 100° C. and then for 2 hours at 120° C. The reaction mixture was poured into water and this mixture was extracted with diisopropyl ether. The separated organic layer was dried, filtered and the solvent evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2:CH3OH 100:0 (to remove unreacted 4-chloro-2-dimethoxymethyl-1-nitrobenzene) up to 70:30). The desired fractions were collected and the solvent was evaporated to yield a residue.

1. waitfor 2 hours at 120° C
2. extractionthis mixture was extracted with diisopropyl ether
3. customThe separated organic layer was dried
4. filtrationfiltered
5. customthe solvent evaporated
6. customThe residue was purified by column chromatography over silica gel (eluent
7. customThe desired fractions were collected
8. customthe solvent was evaporated
9. customto yield a residue