反应 #833564

ord-aab491655b5d4278b1afbed5d1d9d88a

反应方程式

CC#CCn1c(Cl)nc(C(=O)OC)c1C(=O)N(Cc1ccc2ccccc2n1)NC(=O)OC(C)(C)C
methyl 2-chloro-5-[N′-tert-butoxycarbonyl-N-(quinolin-2-ylmethyl)-hydrazinocarbonyl]-1-(but-2-ynyl)-1H-imidazol-4-carboxylate
Cl
hydrochloric acid
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

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度Then the solution is cooled to ambient temperature
  2. 2
    其他the precipitate formed
  3. 3
    其他is separated off
  4. 4
    洗涤washed with ethyl acetate and diethyl ether
  5. 5
    其他dried in the drying cupboard at 50° C.

实验过程

2.80 g methyl 2-chloro-5-[N′-tert-butoxycarbonyl-N-(quinolin-2-ylmethyl)-hydrazinocarbonyl]-1-(but-2-ynyl)-1H-imidazol-4-carboxylate are dissolved in 50 ml of ethyl acetate. Then 1.5 ml of 4 M hydrochloric acid in dioxane are added, and the solution is stirred for 2 h at 50° C. Then the solution is cooled to ambient temperature, the precipitate formed is separated off, washed with ethyl acetate and diethyl ether and dried in the drying cupboard at 50° C.

来源

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