反应详情

14 gm of the compound prepared in (7) above was dissolved into 100 ml of concentrated sulfuric acid. After cooling the solution, a solution of 9.05 gm of potassium nitrate in 80 ml of concentrated sulfuric acid was added dropwise while maintaining the internal temperature below 5° C. The stirring was continued for a further 30 minutes. The resultant reaction mixture was poured into ice-cooled water and extracted with chloroform. The extract was washed with saturated aqueous solution of sodium bicarbonate, water, and saturated brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated and residue was recrystallized in methanol to obtain 9.15 gm of the title compound.

1. temperatureAfter cooling the solution
2. temperaturewhile maintaining the internal temperature below 5° C
3. customThe resultant reaction mixture
4. additionwas poured into ice-
5. extractionextracted with chloroform
6. washThe extract was washed with saturated aqueous solution of sodium bicarbonate, water, and saturated brine in this order
7. dry with materialdried over anhydrous sodium sulfate
8. customThe solvent was evaporated
9. customresidue was recrystallized in methanol