Sodium Methoxide → Pyrimidine, 2-(6-bromo-2-pyridinyl)-4-methyl-
반응식
Cl.[Br:2][C:3]1[N:8]=[C:7]([C:9]([NH2:11])=[NH:10])[CH:6]=[CH:5][CH:4]=1.C[O-].[Na+]>CO.COC(OC)CC(=O)C>[Br:2][C:3]1[N:8]=[C:7]([C:9]2[N:11]=[C:5]([CH3:6])[CH:4]=[CH:3][N:10]=2)[CH:6]=[CH:5][CH:4]=1참가 물질
5
실험 절차
To a mixture of 6-bromo-2-picoline amidine hydrochloride (10 g) and methanol (200 ml) were added 28% sodium methoxide solution in methanol (10.6 g) and 1,1-dimethoxy-3-butanone (6.1 g). The mixture was heated under refluxing for an hour, and then concentrated under reduced pressure. Water (100 ml) and ethylacetate (200 ml) were added thereto, and then extracted. After the extract was dried over anhydrous magnesium sulfate, it was concentrated under reduced pressure. The residue was washed with n-hexane to obtain 2-(6-bromo-2-pyridinyl)-4-methylpyrimidine (8.9 g, yield 84%).
후처리
- temperatureThe mixture was heated
- temperatureunder refluxing for an hour
- concentrationconcentrated under reduced pressure
- additionWater (100 ml) and ethylacetate (200 ml) were added
- extractionextracted
- dry with materialAfter the extract was dried over anhydrous magnesium sulfate, it
- concentrationwas concentrated under reduced pressure
- washThe residue was washed with n-hexane
출처 및 근거
- ORD 기록
- ord-101224141eff419787a9beb4f61385a6
- 출처 데이터셋
- uspto-grants-1990_05
- 특허 번호
- US04927827
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