反应 #1687663

ord-d7c35d4bc4eb4ea6bb7ac196aecb1d8a

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux for 18 h
  2. 2
    其他precipitated out of solution
  3. 3
    过滤The solid was collected by filtration
  4. 4
    其他dried in vacuo

实验过程

A solution of 1-(5-bromopyridin-2-yl)-piperazine (310 mg,1.28 mmol) (prepared in Example 3(b)) and 3-(N,N-dimethylaminomethyl)-1H-pyrrolo[2,3-b]pyridine (215 mg, 1.16 mmol) (prepared in Example 1(a)) in toluene (10 mL) was heated at reflux for 18 h. The heating was discontinued and the solution allowed to cool to room temperature during which time a colourless solid precipitated out of solution. The solid was collected by filtration and dried in vacuo to yield 3-[4-(5-bromopyridin-2-yl)-piperazin-1-yl]methyl-1H-pyrrolo[2,3-b]pyridine as a colourless solid (420 mg, 97%). δH (300 mhz CDCl3) 2.58 (4H, m, piperazinyl), 3.51 (4H, m, piperazinyl), 3.75 (2H, s), 6.50 (1H, d, J=9.0), 7.09 (1H, dd, J=5.0 and 7.9), 7.27 (1H, s), 7.49 (1H, dd, J=2.6 and 9.0), 8.10 (1H, d, J=7.8), 8.17 (1H, d, J=2.3), 8.32 (4.5), 9.69 (1H , br s) ESMS 374 (MH+)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05976497uspto-grants-1999_11