Potassium Carbonate → HCID 11241368, 화합물
반응식
C([CH:3]([C:11]1[CH:16]=[C:15]([CH3:17])[CH:14]=[CH:13][N:12]=1)[C:4]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][CH:5]=1)#N.C(=O)([O-])[O-:19].[K+].[K+]>O>[F:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([C:11]2[CH:16]=[C:15]([CH3:17])[CH:14]=[CH:13][N:12]=2)=[O:19])=[CH:5][CH:6]=1참가 물질
4
실험 절차
2-(α-cyano-4-fluorobenzyl)-4-methylpyridine (3.1 g) and potassium carbonate (2.9 g) were suspended in 20% hydrated dimethylsulfoxide (150 ml), and the suspension was stirred overnight. The mixture was poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and then, the solvent was distilled off. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane), to give 2-(4-fluorobenzoyl)-4-methylpyridine (1.6 g) as brown crystals.
후처리
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off
- customThe residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane)
출처 및 근거
- ORD 기록
- ord-11ac5fb20da64060929094e6d82c09f0
- 출처 데이터셋
- uspto-grants-2007_08
- 특허 번호
- US07262185B2
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