反応 #2290143

反応方程式

1-(2-cyclopropyl-3-methylimidazo[1,2-a]pyridin-6-yl)-4-hydroxypyridin-2(1H)-one

(5-chloro-2-thienyl)methanol

tributylphosphine

1,1′-(azodicarbonyl)dipiperidine

→

title compound

収率 3.2%

4-((5-Chloro-2-thienyl)methoxy)-1-(2-cyclopropyl-3-methylimidazo[1,2-a]pyridin-6-yl)pyridin-2(1H)-one

収率 3.2%

溶媒

THF

反応条件

後処理

1. 1
   温度The reaction mixture was then cooled to room temperature
2. 2
   濃縮concentrated in vacuo
3. 3
   workup.ADDITIONThe residue was diluted with DCM
4. 4
   洗浄washed with water and brine
5. 5
   乾燥dried over Na2SO4
6. 6
   濃縮concentrated in vacuo
7. 7
   その他The residue was purified by silica gel column chromatography (MeOH/DCM)

実験手順

To a solution of 1-(2-cyclopropyl-3-methylimidazo[1,2-a]pyridin-6-yl)-4-hydroxypyridin-2(1H)-one (150 mg), (5-chloro-2-thienyl)methanol (158 mg) and tributylphosphine (322 mg) in THF (15 ml) was added 1,1′-(azodicarbonyl)dipiperidine (401 mg). The mixture was stirred under sonication at 60° C. for 4 h. The reaction mixture was then cooled to room temperature, and concentrated in vacuo. The residue was diluted with DCM, washed with water and brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (MeOH/DCM) to give the title compound (7 mg) as a white solid.

出典