反应详情

温度

190 °C

6-Bromo-2-naphthol (2.0 g, 9 mmol), ammonium sulfite (10.4 g, 90 mmol) and 10 mL of ammonia solution were sealed in a tube. The reaction mixture was heated at 190° C. for 24 hrs and allowed to cool to room temperature, the reaction mixture was extracted with EtOAc. HCl (10%) was added to the organic layer to give a precipitate. After filtration, the solid was dissolved in 10% of Na2CO3 and extracted with EtOAc, the organic layer was dried over Na2SO4. The solvent was removed under reduced pressure to give the product as yellow solid (0.67 g, 33%). MS [M++43]=265, LC-MS: tR=2.14 min.

1. temperatureto cool to room temperature
2. extractionthe reaction mixture was extracted with EtOAc
3. additionHCl (10%) was added to the organic layer
4. customto give a precipitate
5. filtrationAfter filtration
6. dissolutionthe solid was dissolved in 10% of Na2CO3
7. extractionextracted with EtOAc
8. dry with materialthe organic layer was dried over Na2SO4
9. customThe solvent was removed under reduced pressure