反応 #2290157

反応方程式

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

(5-fluorothiophen-2-yl)methanol

potassium tert-butoxide

potassium tert-butoxide

(5-fluorothiophen-2-yl)methanol

→

title compound

収率 36.8%

1-(2-Cyclopropyl-3-methylimidazo[1,2-a]pyridin-6-yl)-4-((5-fluorothiophen-2-yl)methoxy)pyridin-2(1H)-one

収率 36.8%

溶媒

DME

DME

反応条件

後処理

1. 1
   温度the resulting mixture was heated at 120° C. for further 30 min under microwave irradiation
2. 2
   その他The mixture was quenched with water
3. 3
   抽出extracted with EtOAc/MeOH
4. 4
   その他The organic layer was separated
5. 5
   洗浄washed with brine
6. 6
   乾燥dried over MgSO4
7. 7
   濃縮concentrated in vacuo
8. 8
   その他The resulting solid was crystallized from EtOH-IPA

実験手順

A mixture of 4-bromo-1-(2-cyclopropyl-3-methylimidazo[1,2-a]pyridin-6-yl)pyridin-2(1H)-one (285 mg), (5-fluorothiophen-2-yl)methanol (109 mg), potassium tert-butoxide (93 mg) and DME (5 ml) was heated at 120° C. for 30 min under microwave irradiation. Additional potassium tert-butoxide (93 mg) and (5-fluorothiophen-2-yl)methanol (109 mg) in DME (0.5 ml) were added to the reaction mixture, and the resulting mixture was heated at 120° C. for further 30 min under microwave irradiation. The mixture was quenched with water and extracted with EtOAc/MeOH. The organic layer was separated, washed with brine, dried over MgSO4 and concentrated in vacuo. The resulting solid was crystallized from EtOH-IPA to give the title compound (120 mg) as an off-white solid.

出典