반응 #1943

반응 방정식

Ethyl 8-chloro-4H-quinolizin-4-one-3-carboxylate

product

Ethyl 8-chloro-4H-quinolizin-4-one-3-carboxylate

N-methylpiperazine

→

title compound

수율 106.8%

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

수율 106.8%

용매

pyridine

반응 조건

후처리

1. 1
   농축The reaction mixture was then concentrated in vacuo in order
2. 2
   기타to remove all of the pyridine
3. 3
   workup.DISSOLUTIONThe dry residue (3.124 g) was dissolved in 125 mL of methylene chloride
4. 4
   세척the methylene chloride solution was washed with 125 mL of saturated sodium chloride solution (brine)
5. 5
   추출The aqueous layer was extracted with 125 mL of methylene chloride
6. 6
   건조the combined methylene chloride solutions were dried over anhydrous sodium sulfate
7. 7
   여과filtered
8. 8
   농축concentrated
9. 9
   기타dried in vacuo

실험 절차

Ethyl 8-chloro-4H-quinolizin-4-one-3-carboxylate (755 mg, 3.0 mmol), the product of Step 3 of Example 58, was suspended in 12 mL of dry pyridine under a nitrogen atmosphere. To the resultant solution was added 6.0 mL (6.0 mmol) of N-methylpiperazine and the reaction mixture was heated at 70° C. for 8 hours. The reaction mixture was then concentrated in vacuo in order to remove all of the pyridine. The dry residue (3.124 g) was dissolved in 125 mL of methylene chloride and the methylene chloride solution was washed with 125 mL of saturated sodium chloride solution (brine). The aqueous layer was extracted with 125 mL of methylene chloride and the combined methylene chloride solutions were dried over anhydrous sodium sulfate, filtered and concentrated and dried in vacuo to afford 1.01 g of the title compound.

출처