反应详情

温度

50 °C

Ethyl-3-amino-5-methyl-1H-pyrrole-2-carboxylate (58.87 g; 0.35 mol) prepared according to literature [Gangjee A.; Li W.; Yang J.; Kisliuk R. L.; J. Med. Chem. 2008, 51, 68] is suspended in acetonitrile (1750 mL). To the suspension is added dropwise 4M HCl in dioxane (473 mL; 1.89 mol) within 15 minutes. After complete addition the reaction mixture is heated to 50° C. for 18 hours. The reaction mixture is cooled to 10° C., the solid is collected by suction filtration and washed with cold acetonitrile (400 mL). A second crop of product is obtained from the mother liquor after concentration under reduced pressure. The residue is collected with t-butylmethyl-ether. After the suction filtration the solids are combined and dried in vacuum at 50° C. to yield the title compound as off-white solid.

1. additionAfter complete addition the reaction mixture
2. temperatureThe reaction mixture is cooled to 10° C.
3. filtrationthe solid is collected by suction filtration
4. washwashed with cold acetonitrile (400 mL)
5. customA second crop of product is obtained from the mother liquor
6. concentrationafter concentration under reduced pressure
7. customThe residue is collected with t-butylmethyl-ether
8. filtrationAfter the suction filtration the solids
9. customdried in vacuum at 50° C.