反应 #89436

ord-e335bafc470c432e895b59949de942d2

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was cooled to rt
  2. 2
    过滤filtered through diatomaceous earth
  3. 3
    其他The solvent was removed
  4. 4
    其他the crude residue was purified via silica gel chromatography

实验过程

A mixture of ((2S,3R)-2-(((5-bromoquinazolin-2-yl)amino)methyl)-3-methylpiperidin-1-yl)(5-methyl-2-(2H-1,2,3-triazol-2-yl)phenyl)methanone (0.057 g, 0.111 mmol), HCOONH4 (0.14 g, 0.222 mmol) and Pd(PPh3)4 (0.026 g, 0.022 mmol) in dioxane and water (4:1, 2 mL) was heated for 2 h at 100° C. The mixture was cooled to rt and filtered through diatomaceous earth. The solvent was removed and the crude residue was purified via silica gel chromatography to obtain the title compound. ESI-MS (m/z): 442 [M+1]+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09440982B2uspto-grants-2016_09