반응 #165016

ord-9bfab83f2eb7466e9bc8c3324ee34706

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

To a solution of 3-trimethylsilanylethynyl-pyridin-2,6-diamine (7.0 g, 34.1 mmoL) described in Manufacturing Example 13-1-2 in tetrahydrofuran (100 mL) was added tetrabutylammonium fluoride (1M tetrahydrofuran solution, 17 mL, 17 mmol) on an ice bath, which was stirred for 10 minutes at room temperature. Water was added to the reaction solution, which was then extracted with ethyl acetate 3 times. The extract was dried over sodium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate) to obtain the title compound (3.35 g, 73.8%).

출처

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