反应详情

77 μL (0.925 mmol) of pyrrolidine is added to a solution of 90 mg (0.231 mmol) of 2-chloro-6-[5-(4-chlorophenyl)pyridin-2-ylethynyl]-4-methylquinoline in 5 mL of 1,4-dioxane and the reaction mixture is refluxed overnight. It is evaporated down in vacuo, and the residue is taken up in DMF and purified by HPLC-MS. The fractions containing the product are combined, evaporated down, and freeze-dried. The product is dissolved in DCM, evaporated down, and the residue is triturated with a little EtOAc, filtered, washed again with a little EtOAc, and dried at 50° C. in the circulating air dryer. Yield: 39 mg (39% of theoretical); C27H22ClN3 (M=423.936); calc.: molpeak (M+H)+: 424/426 (Cl); found: molpeak (M+H)+: 424/426 (Cl); HPLC-MS: 5.8 min (method A).

1. temperaturethe reaction mixture is refluxed overnight
2. customIt is evaporated down in vacuo
3. custompurified by HPLC-MS
4. additionThe fractions containing the product
5. customevaporated down
6. customfreeze-dried
7. dissolutionThe product is dissolved in DCM
8. customevaporated down
9. customthe residue is triturated with a little EtOAc
10. filtrationfiltered
11. washwashed again with a little EtOAc
12. customdried at 50° C. in the circulating air dryer
13. custom5.8 min (method A)