반응식
[N:1]1[CH:2]=[CH:3][N:4]2[CH:9]=[C:8]([CH:10]=[O:11])[CH:7]=[CH:6][C:5]=12.[BH4-].[Na+].O.ClCCl.CO>CO>[N:1]1[CH:2]=[CH:3][N:4]2[CH:9]=[C:8]([CH2:10][OH:11])[CH:7]=[CH:6][C:5]=12참가 물질
6
실험 절차
0.90 g of the 6-imidazo[1,2-a]pyridinecarbaldehyde prepared in the Preparative Example 5 was dissolved in 20 ml of methanol. The obtained solution was stirred under cooling with ice, followed by the addition of 90 mg of sodium borohydride. The obtained mixture was stirred for 50 minutes, followed by the addition of water. The obtained mixture was extracted with chloroform. The organic phase was dried over anhydrous magnesium sulfate and distilled to remove the solvent. The obtained residue was purified by silica gel column chromatography [solvent: dichloromethane/methanol (30:1 to 10:1) to give 0.52 g of the title compound as a faintly orange-yellow solid (yield: 57%).
후처리
- temperatureunder cooling with ice
- stirringThe obtained mixture was stirred for 50 minutes
- extractionThe obtained mixture was extracted with chloroform
- dry with materialThe organic phase was dried over anhydrous magnesium sulfate
- distillationdistilled
- customto remove the solvent
- customThe obtained residue was purified by silica gel column chromatography [solvent
출처 및 근거
- ORD 기록
- ord-41af41c29e0942c9ae91c5ee99e256c0
- 출처 데이터셋
- uspto-grants-1996_03
- 특허 번호
- US05498634
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