反应详情

2-phenylazoaniline (3.47 g, 17.6 mmol) prepared above was placed in a 100-mL 1-neck round bottomed flask. Acetic acid (20 mL) and iodobenzene diacetate (6.23 g, 19.4 mmol) were added, in that order, resulting in an exotherm. The reaction was allowed to proceed for 1 hour during which time the mixture cooled to room temperature. Dichloromethane and water were added to the reaction mixture. The organic layer was separated and dried over MgSO4. The solution was filtered and concentrated using a rotary evaporator. The residue was purified on a silica gel column using dichloromethane as eluent. The fractions containing the desired product were combined and solvent removed. The solid was dried in a vacuum oven for 2 h. Yield: 34%.

1. customresulting in an exotherm
2. customThe organic layer was separated
3. dry with materialdried over MgSO4
4. filtrationThe solution was filtered
5. concentrationconcentrated
6. customa rotary evaporator
7. customThe residue was purified on a silica gel column
8. additionThe fractions containing the desired product
9. customsolvent removed
10. customThe solid was dried in a vacuum oven for 2 h