Methyl iodide → HCID 59463819、化合物
反応式
[Br:1][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5](=[O:12])[NH:4][CH:3]=1.[CH3:13]I>C(Cl)(Cl)Cl.C(=O)([O-])[O-].[Ag+].[Ag+]>[Br:1][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]([O:12][CH3:13])=[N:4][CH:3]=1参加物
5
反応条件
- 温度
- 50 °C
実験手順
47.7 g (209 mmol) of 4-bromo-5,6,7,8-tetrahydro-2H-isoquinolin-1-one are dissolved in 1 l of chloroform and, after addition of 77.8 g (282 mmol) of silver(I) carbonate and 53.5 ml (118.7 g, 836 mmol) of methyl iodide, stirred at 50° C. for 3 h. After cooling, the suspension is filtered through Celite, concentrated and chromatographed on silica gel using n-heptane with addition of 2% ethyl acetate. A colorless oil (42.5 g, 84% yield) is obtained.
後処理
- temperatureAfter cooling
- filtrationthe suspension is filtered through Celite
- concentrationconcentrated
- customchromatographed on silica gel
- additionwith addition of 2% ethyl acetate
出典と根拠
- ORDレコード
- ord-7fb22eb221004955a6bad02614f70010
- 出典データセット
- uspto-grants-2010_09
- 特許番号
- US07795278B2
反応ノート
読み込み中…