反応 #833565

反応方程式

sodium chloride

1-(but-2-ynyl)-2-chloro-6-(quinolin-2-ylmethyl)-5,6-dihydro-1H-imidazo[4,5-d]-pyridazine-4,7-dione

potassium carbonate

bromoacetonitrile

→

1-(but-2-ynyl)-2-chloro-5-cyanomethyl-6-(quinolin-2-ylmethyl)-5,6-dihydro-1H-imidazo[4,5-d]pyridazine-4,7-dione

溶媒

dimethylformamide

反応条件

後処理

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

実験手順

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).

出典