Sodium Methoxide → Pyrimidine, 2-(6-bromo-2-pyridinyl)-4-methyl-
反応式
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]=1参加物
5
実験手順
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%).
後処理
- 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
出典と根拠
- ORDレコード
- ord-101224141eff419787a9beb4f61385a6
- 出典データセット
- uspto-grants-1990_05
- 特許番号
- US04927827
反応ノート
読み込み中…