反应详情

温度

105 °C

A mixture of 150 mg (0.34 mmol) of 4-[3-chloro-4-(1-methyl-1H-imidazole-2-ylsulfanyl)-phenylamino]-7-fluoro-6-methoxyquinoline-3-carbonitrile and 316 mg (2.05 mmol) of 4-pyrrolidin-1-yl-piperidine in 1 mL of 1-methyl-2-pyrrolidinone is heated at 105° C. for 16 hours. The solvents are removed in vacuo. A 10 mL portion of water is added to the residue, from which a tan solid is precipitated out. The solid is filtered off and washed with water. After drying in vacuo, the solid is suspended in ethyl acetate and stirred for 1 hour. The solid is filtered off, washed with ethyl acetate and dried in vacuo to provide 140 mg of 4-[3-chloro-4-(1-methyl-1H-imidazole-2-ylsulfanyl)-phenylamino]-6-methoxy-7-(4-pyrrolidin-1-yl-piperidin-1-yl)-quinoline-3-carbonitrile as a yellow solid, mp 225-229° C.

1. customThe solvents are removed in vacuo
2. additionA 10 mL portion of water is added to the residue, from which a tan solid
3. customis precipitated out
4. filtrationThe solid is filtered off
5. washwashed with water
6. customAfter drying in vacuo
7. filtrationThe solid is filtered off
8. washwashed with ethyl acetate
9. customdried in vacuo