Thionyl Chloride → 2,4-Dimethylpyridin-3-amine
反応式
[CH3:1][C:2]1[N:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:3]=1C(O)=O.S(Cl)(Cl)=O.[N-:16]=[N+]=[N-].[Na+]>O>[CH3:1][C:2]1[C:3]([NH2:16])=[C:7]([CH3:11])[CH:8]=[CH:9][N:10]=1参加物
5
反応条件
- 温度
- 60 °C
実験手順
A mixture of 1a (0.98 g, 6.5 mmol) and thionyl chloride (5 ml) was heated to 60° C. for 1 hour. The mixture was concentrated to dryness. The mixture was then dissolved in acetone (10 ml) prior to the addition of NaN3 (0.65 g, 10 mmol) and water (5 ml). The solution was heated to 70° C. for 1 hour. Acetone was evaporated from the reaction mixture which was washed with brine and extracted with ethyl acetate. The organic layer was dried over MgSO4, concentrated and chromatographed to yield 1b (0.585 g, 4.79 mmol, 74%).
後処理
- concentrationThe mixture was concentrated to dryness
- dissolutionThe mixture was then dissolved in acetone (10 ml)
- temperatureThe solution was heated to 70° C. for 1 hour
- customAcetone was evaporated from the reaction mixture which
- washwas washed with brine
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated
- customchromatographed
出典と根拠
- ORDレコード
- ord-161e9a64b288476da7e8ad850f7924be
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08367684B2
反応ノート
読み込み中…