Methyl iodide → 3-Bromo-5-ethyl-6-methoxy-2-methylpyridine
反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:10][CH3:11])[C:5](=[O:9])[NH:6][C:7]=1[CH3:8].[CH3:12]I>C(Cl)(Cl)Cl.C(=O)([O-])[O-].[Ag+2]>[Br:1][C:2]1[C:7]([CH3:8])=[N:6][C:5]([O:9][CH3:12])=[C:4]([CH2:10][CH3:11])[CH:3]=1参加物
5
実験手順
5-Bromo-3-ethyl-6-methyl-1H-pyridin-2-one (25 g, 115.7 mmol) was dissolved in 200 ml of chloroform to form an orange solution. Silver carbonate (31.9 g, 115.7 mmol) was added and the mixture was vigorously stirred. Methyl iodide (10.8 ml, 1.5 mmol) was added to this suspension, which was then stirred in the dark at RT under nitrogen. After 3 days, the mixture was filtered and the solution was concentrated in a rotary evaporator. The residue was chromatographed on silica gel with n-heptane as mobile phase and afforded a colorless oil (21.7 g, 82%).
後処理
- customto form an orange solution
- stirringwas then stirred in the dark at RT under nitrogen
- filtrationthe mixture was filtered
- concentrationthe solution was concentrated in a rotary evaporator
- customThe residue was chromatographed on silica gel with n-heptane as mobile phase
出典と根拠
- ORDレコード
- ord-b6c79297801249f9ad8abeff96178557
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07863280B2
反応ノート
読み込み中…