反应 #833565

ord-5372f06f6e474f9fbf0181ed047b82f0

反应方程式

[Cl-].[Na+]
sodium chloride
CC#CCn1c(Cl)nc2c(=O)[nH]n(Cc3ccc4ccccc4n3)c(=O)c21
1-(but-2-ynyl)-2-chloro-6-(quinolin-2-ylmethyl)-5,6-dihydro-1H-imidazo[4,5-d]-pyridazine-4,7-dione
O=C([O-])[O-].[K+].[K+]
potassium carbonate
N#CCBr
bromoacetonitrile
CC#CCn1c(Cl)nc2c(=O)n(CC#N)n(Cc3ccc4ccccc4n3)c(=O)c21
1-(but-2-ynyl)-2-chloro-5-cyanomethyl-6-(quinolin-2-ylmethyl)-5,6-dihydro-1H-imidazo[4,5-d]pyridazine-4,7-dione

反应条件

温度
40°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取is extracted three times with ethyl acetate
  2. 2
    干燥the combined organic phases are dried over sodium sulphate
  3. 3
    其他the solvent is removed
  4. 4
    其他The residue is purified over silica gel (cyclohexane/ethyl acetate 1:1)

实验过程

0.20 g 1-(but-2-ynyl)-2-chloro-6-(quinolin-2-ylmethyl)-5,6-dihydro-1H-imidazo[4,5-d]-pyridazine-4,7-dione and 0.25 g potassium carbonate are placed in 4 ml of dimethylformamide. Then 53 μl of bromoacetonitrile are added and the mixture is stirred for 2 h at 40° C. After the addition of aqueous saturated sodium chloride solution the mixture is extracted three times with ethyl acetate, the combined organic phases are dried over sodium sulphate, and then the solvent is removed. The residue is purified over silica gel (cyclohexane/ethyl acetate 1:1).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07393847B2uspto-grants-2008_07