반응 #833565

ord-5372f06f6e474f9fbf0181ed047b82f0

반응 방정식

[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

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출is extracted three times with ethyl acetate
  2. 2
    건조the combined organic phases are dried over sodium sulphate
  3. 3
    기타the solvent is removed
  4. 4
    기타The residue is purified over silica gel (cyclohexane/ethyl acetate 1:1)

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07393847B2uspto-grants-2008_07