반응 #89436

ord-e335bafc470c432e895b59949de942d2

반응 조건

온도
100°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was cooled to rt
  2. 2
    여과filtered through diatomaceous earth
  3. 3
    기타The solvent was removed
  4. 4
    기타the crude residue was purified via silica gel chromatography

실험 절차

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]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440982B2uspto-grants-2016_09