反应 #1860827

ord-da6a2e1f1ea2434f91af482b3e2153a5

溶剂

反应条件

温度
120°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他was prepared
  2. 2
    萃取extracted with a mixture of dichloromethane and methanol
  3. 3
    干燥The combined organic phases were dried over sodium sulfate
  4. 4
    过滤After filtration and removal of solvent the residue
  5. 5
    其他was purified by chromatography

实验过程

A mixture of 28.0 mg (53 μmol) N-cyclopropyl-4-{6-(2-methoxyphenoxy)-8-[(3,3,3-trifluoropropyl)amino]imidazo[1,2-b]pyridazin-3-yl}-2-methylbenzamide which was prepared according to example 223, 44.8 mg sodium methanethiolate and 350 μL N,N-dimethylformamide was heated under microwave irradiation for 30 minutes at 120° C. The mixture was poured into water, the pH was adjusted between 7 and 8 by addition of ammonium chloride and extracted with a mixture of dichloromethane and methanol. The combined organic phases were dried over sodium sulfate. After filtration and removal of solvent the residue was purified by chromatography to give 11.5 mg (40%) of the title compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09255100B2uspto-grants-2016_02