反应详情

AIBN (84 mg, 0.51), NBS (1.1 gram, 6.4 mmol), and the methyl 2-methyl-4-nitrobenzoate (1 g, 5.1 mmol) from step 1 of this example were suspended in CCl4 and the mixture heated under N2 at 79 C overnight. The solution was filtered, and concentrated in vacuum. The residue was dissolved in 7 N ammonia in methanol (15 ml) and the solution stirred for 2 hours at RT. The mixture was concentrated in vacuum. and the resulting solid suspended in EtOAc (21.5 ml), heated at 80° C. for 30 minutes with stirring, cooled RT and aged at −20° C. for the 3 days. The solid was isolated by filtration to give the titled compound.

1. temperaturethe mixture heated under N2 at 79 C overnight
2. filtrationThe solution was filtered
3. concentrationconcentrated in vacuum
4. dissolutionThe residue was dissolved in 7 N ammonia in methanol (15 ml)
5. concentrationThe mixture was concentrated in vacuum
6. temperatureheated at 80° C. for 30 minutes
7. stirringwith stirring
8. temperaturecooled RT
9. customaged at −20° C. for the 3 days
10. customThe solid was isolated by filtration