反应详情

To a mixture of 4-hydroxy-3-methoxy-2-nitrobenzaldehyde 14.5 g (73.5 mmol) in 28% ammonia solution 150 mL and tetrahydrofuran 15 mL was added iodine 22.4 g (88.2 mmol) and stirred at room temperature for overnight. The reaction mixture was concentrated in vacuo. The residue was acidified with 2H HCl solution and extracted into diethyl ether. The organic layer was washed with brine, dried over MgSO4, filtrated and the solvent was evaporated. The residue was washed with diisopropyl ether to give the title compound 12.1 g as brown solid. Yield 84.5%

1. concentrationThe reaction mixture was concentrated in vacuo
2. extractionextracted into diethyl ether
3. washThe organic layer was washed with brine
4. dry with materialdried over MgSO4
5. filtrationfiltrated
6. customthe solvent was evaporated
7. washThe residue was washed with diisopropyl ether