Sodium Methoxide → 7-Bromo-2-methoxymethylimidazo[1,2-a]pyridine
반응식
[Br:1][C:2]1[CH:7]=[CH:6][N:5]2[CH:8]=[C:9]([CH2:11]Cl)[N:10]=[C:4]2[CH:3]=1.[CH3:13][O-:14].[Na+]>CO>[Br:1][C:2]1[CH:7]=[CH:6][N:5]2[CH:8]=[C:9]([CH2:11][O:14][CH3:13])[N:10]=[C:4]2[CH:3]=1참가 물질
실험 절차
To a solution of 81 mg (0.33 mmol) of 7-bromo-2-chloromethylimidazo[1,2-a]pyridine, prepared according to the protocol described in step 8.3, in 3 mL of anhydrous methanol, stirred at room temperature under an inert atmosphere, are added 35 mg (0.99 mmol) of sodium methoxide. The reaction mixture is stirred at 100° C. for 4 hours. After this time, the reaction medium, cooled to room temperature, is concentrated under reduced pressure, diluted with 10 mL of chloroform and then washed with 10 mL of saturated aqueous NaCl solution. The crude reaction product obtained after evaporating off the solvent under reduced pressure is purified by chromatography on a column of silica gel, eluting with a mixture of dichloromethane and methanol. 27 mg of the expected product are thus obtained.
후처리
- stirringThe reaction mixture is stirred at 100° C. for 4 hours
- temperatureAfter this time, the reaction medium, cooled to room temperature
- concentrationis concentrated under reduced pressure
- additiondiluted with 10 mL of chloroform
- washwashed with 10 mL of saturated aqueous NaCl solution
- customThe crude reaction product
- customobtained
- customafter evaporating off the solvent under reduced pressure
- customis purified by chromatography on a column of silica gel
- washeluting with a mixture of dichloromethane and methanol
출처 및 근거
- ORD 기록
- ord-c40d237243de4f9cac7b1f86d590f0ca
- 출처 데이터셋
- uspto-grants-2013_03
- 특허 번호
- US08394820B2
반응 노트
불러오는 중…