反应详情

A solution of 2.21 g of 2-chloro-5-nitronicotinoyl chloride (obtained by nitrating 2-hydroxynicotinic acid, followed by conversion to 2-chloro-5-nitronicotinic acid, which was then treated with thionyl chloride) in 10 ml of tetrahydrofuran was slowly added over 15 minutes to a cooled, stirred mixture of 1.34 g of 3-Amino-2-ethylaminopyridine, 1.29 g of diisopropylethylamine, and 40 ml of tetrahydrofuran. The resulting mixture was allowed to stir overnight at room temperature, and then concentrated in vacuo. The title compound (2.30 g, m.p. 185°-186° C.), which precipitated out when the residue was treated with methylene chloride, was suitable for use in the next reaction.

1. additionwas slowly added over 15 minutes to a cooled
2. stirringto stir overnight at room temperature
3. concentrationconcentrated in vacuo
4. customThe title compound (2.30 g, m.p. 185°-186° C.), which precipitated out when the residue
5. additionwas treated with methylene chloride
6. customwas suitable for use in the next reaction