反应详情

温度

100 °C

15 g of 2,6-dichloronicotinic acid (70.31 mmol, Aldrich) and 34.7 ml of cyclopentylamine (351.56 mmol) are placed in a sealed tube containing 40 ml of tert-butanol. The mixture is heated at 100° C. overnight and evaporated to dryness. The residue is taken up in water and the product is acidified by pouring in an aqueous solution of acetic acid at 10%, and the mixture is then extracted with choloroform. The organic phases are combined, dried over sodium sulphate, filtered, and concentrated under vacuum. The solid residue is triturated in an ether/pentane mixture so as to give 5 g of expected product in the form of an off-white solid (yield=29.5%).

1. customevaporated to dryness
2. additionby pouring in an aqueous solution of acetic acid at 10%
3. extractionthe mixture is then extracted with choloroform
4. dry with materialdried over sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe solid residue is triturated in an ether/pentane mixture so as