反应详情

The compound of example 1 (3.4 g) was dissolved in ethanol (40 ml) and diluted hydrochloric acid (20 ml) and reduced over a Pd catalyst (5% on carbon) under H2 pressure (50 psi) in a Parr apparatus. Water (20 ml) was added and the catalyst filtered off. The resulting solution was concentrated and the residue was dissolved in water (40 ml). Sodium bicarbonate (4 g) was added, followed by a solution of N-methyl-4-nitropyrrole-2-carboxylic acid chloride (2.8 g) in 20 ml of benzene. The resulting mixture was stirred for about 2 hours at room temperature and then was extracted with chloroform. The dried organic extracts were concentrated in vacuo and the residue was purified by column chromatography (CHCl3 75, EtOH95% 25, NH4OH 0.6) to give 4.7 g of 3-[N-methyl-4-(N-methyl-4-nitropyrrole-2-carboxamido)pyrrole-2-carboxamido]propyl-dimethylamine as a yellow solid, m.p. 178°-180° C.

1. filtrationthe catalyst filtered off
2. concentrationThe resulting solution was concentrated
3. dissolutionthe residue was dissolved in water (40 ml)
4. additionSodium bicarbonate (4 g) was added
5. extractionwas extracted with chloroform
6. concentrationThe dried organic extracts were concentrated in vacuo
7. customthe residue was purified by column chromatography (CHCl3 75, EtOH95% 25, NH4OH 0.6)