반응 #164978

ord-28557e6571f64d84b8e6524cf1f92b12

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출was then extracted with ethyl acetate 4 times
  2. 2
    건조The organic layer was dried over anhydrous sodium sulfate
  3. 3
    기타the solvent was evaporated under a reduced pressure
  4. 4
    기타The residue was purified by silica gel chromatography (heptane

실험 절차

To a solution of 3-trimethylsilanylethynyl-pyridin-2-ylamine (28.1 g, 148 mmoL) described in Manufacturing Example 1-2-2 in tetrahydrofuran (300 mL) was added tetrabutylammonium fluoride (1 M tetrahydrofuran solution, 20 mL, 20 mmol), which was stirred for 15 minutes at room temperature. Water was added to the reaction solution, which was then extracted with ethyl acetate 4 times. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel chromatography (heptane:ethyl acetate=1:1 then 1:2) to obtain the title compound (16.4 g, 93.7%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08841327B2uspto-grants-2014_09