反応 #2290169

反応方程式

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

(4-chlorothiophen-2-yl)methanol

tributylphosphine

1,1′-(azodicarbonyl)dipiperidine

→

title compound

収率 5.5%

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

収率 5.5%

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 (100 ml)
4. 4
   洗浄washed with water and brine successively
5. 5
   乾燥dried over Na2SO4
6. 6
   濃縮concentrated in vacuo
7. 7
   その他The crude product 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), (4-chlorothiophen-2-yl)methanol (158 mg) and tributylphosphine (322 mg) in THF (15 ml) was added 1,1′-(azodicarbonyl)dipiperidine (400 mg), and the mixture was stirred 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 (100 ml), washed with water and brine successively, dried over Na2SO4, and concentrated in vacuo. The crude product was purified by silica gel column chromatography (MeOH/DCM) to afford the title compound (12 mg) as a white solid.

出典