反应详情

Cyclopropanemethylamine (1.70 g, 23.90 mmol) was added to a solution of 6-chloro-5-nitronicotinic acid (1.12 g, 5.53 mmol) in MeOH (25 mL) at room temperature. The reaction mixture was stirred at room temperature for 2 h and concentrated in vacuo. The residue was dissolved in H2O (20 mL), and the solution was acidified by adding 3N HCl until pH=3. The mixture was extracted with EtOAc and CH2Cl2 (2×100 mL) and the combined extracts were washed with brine, dried over Na2SO4, concentrated in vacuo to give a bright yellow solid (1.30 g) which was used in the following reaction without further purification.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in H2O (20 mL)
3. additionby adding 3N HCl until pH=3
4. extractionThe mixture was extracted with EtOAc and CH2Cl2 (2×100 mL)
5. washthe combined extracts were washed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo