反应 #1943

ord-d1417262cbeb4dcfb27be135b8b405b2

溶剂

反应条件

温度
70°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩The reaction mixture was then concentrated in vacuo in order
  2. 2
    其他to remove all of the pyridine
  3. 3
    workup.DISSOLUTIONThe dry residue (3.124 g) was dissolved in 125 mL of methylene chloride
  4. 4
    洗涤the methylene chloride solution was washed with 125 mL of saturated sodium chloride solution (brine)
  5. 5
    萃取The aqueous layer was extracted with 125 mL of methylene chloride
  6. 6
    干燥the combined methylene chloride solutions were dried over anhydrous sodium sulfate
  7. 7
    过滤filtered
  8. 8
    浓缩concentrated
  9. 9
    其他dried in vacuo

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726182uspto-grants-1998_03