反应 #1943
ord-d1417262cbeb4dcfb27be135b8b405b2
反应方程式
反应物
试剂
溶剂
反应条件
后处理
- 1浓缩The reaction mixture was then concentrated in vacuo in order
- 2其他to remove all of the pyridine
- 3workup.DISSOLUTIONThe dry residue (3.124 g) was dissolved in 125 mL of methylene chloride
- 4洗涤the methylene chloride solution was washed with 125 mL of saturated sodium chloride solution (brine)
- 5萃取The aqueous layer was extracted with 125 mL of methylene chloride
- 6干燥the combined methylene chloride solutions were dried over anhydrous sodium sulfate
- 7过滤filtered
- 8浓缩concentrated
- 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.