5-Bromo-4,6-dimethylpyridin-2-amine → HCID 178429301、化合物
反応式
N[C:2]1[CH:7]=[C:6]([CH3:8])[C:5]([Br:9])=[C:4]([CH3:10])[N:3]=1.N([O-])=[O:12].[Na+]>S(=O)(=O)(O)O.O>[Br:9][C:5]1[C:6]([CH3:8])=[CH:7][C:2]([OH:12])=[N:3][C:4]=1[CH3:10]参加物
5
実験手順
2-amino-5-bromo-4,6-dimethylpyridine (15 g) was dissolved in a mixed solution of sulfuric acid (14.2 mL) and water (212 mL). A solution of sodium nitrite (6.18 g) in water (31 mL) was added to the solution at 0° C. The reaction mixture was stirred at mom temperature for one hour, followed by extraction with chloroform. The organic layer was dried over anhydrous magnesium sulfate, and the desiccant was filtered off. The filtrate was concentrated under reduced pressure. MTBE was added to the residue to precipitate the solid, followed by filtration. The filtration residue was washed with MTBE to give the title compound (13.7 g).
後処理
- extractionfollowed by extraction with chloroform
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- filtrationthe desiccant was filtered off
- concentrationThe filtrate was concentrated under reduced pressure
- additionMTBE was added to the residue
- customto precipitate the solid
- filtrationfollowed by filtration
- washThe filtration residue was washed with MTBE
出典と根拠
- ORDレコード
- ord-a776de9b47cf4981b1071060197f4f51
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08563565B2
反応ノート
読み込み中…