反应详情

3,5-Dimethoxyaniline hydrochloride (80.21 g, 0.424 mol) was added cautiously to oxalyl chloride (136 ml, 1.56 mol) and the solution heated at reflux for 3 hours. The solution was cooled and concentrated in vacuo. Methanol (300 ml) was added to the residue and the mixture heated at reflux for 1 hour. The reaction was allowed to cool, and the resulting precipitate filtered and washed with methanol to yield 4,6-dimethoxyisatin (40.4 g, 46%) as a yellow solid.

1. temperaturethe solution heated
2. temperatureat reflux for 3 hours
3. temperatureThe solution was cooled
4. concentrationconcentrated in vacuo
5. additionMethanol (300 ml) was added to the residue
6. temperaturethe mixture heated
7. temperatureat reflux for 1 hour
8. temperatureto cool
9. filtrationthe resulting precipitate filtered
10. washwashed with methanol