반응 #1963

반응 방정식

Ethyl 8-chloro-7-fluoro-1-methylamino-4H-quinolizin-4-one-3-carboxylate

product

Ethyl 8-chloro-7-fluoro-1-methylamino-4H-quinolizin-4-one-3-carboxylate

N-methylpiperazine

→

title compound

Ethyl 7-fluoro-1-methylamino-8-(4-methylpiperazin-1-yl)-4H-quinolizin-4-one-3-carboxylate

용매

pyridine

반응 조건

후처리

1. 1
   농축The reaction mixture is then concentrated in vacuo in order
2. 2
   기타to remove all of the pyridine
3. 3
   workup.DISSOLUTIONThe dry residue is dissolved in 125 mL of methylene chloride
4. 4
   세척the methylene chloride solution is washed with 125 mL of brine
5. 5
   추출The aqueous layer is extracted with 125 mL of methylene chloride
6. 6
   건조the combined methylene chloride solutions are dried over anhydrous sodium sulfate
7. 7
   여과filtered
8. 8
   농축concentrated
9. 9
   기타dried in vacuo

실험 절차

Ethyl 8-chloro-7-fluoro-1-methylamino-4H-quinolizin-4-one-3-carboxylate (899 mg, 3.0 mmol), the product of Step 6, is suspended in 12 mL of dry pyridine under a nitrogen atmosphere. To the resultant solution is added 6.0 mL (6.0 mmol) of N-methylpiperazine and the reaction mixture is heated at 70° C. for 8 hours. The reaction mixture is then concentrated in vacuo in order to remove all of the pyridine. The dry residue is dissolved in 125 mL of methylene chloride and the methylene chloride solution is washed with 125 mL of brine. The aqueous layer is extracted with 125 mL of methylene chloride and the combined methylene chloride solutions are dried over anhydrous sodium sulfate, filtered and concentrated and dried in vacuo to afford the title compound.

출처