Methyl iodide → HCID 10752374、化合物
反応式
[CH3:1][C:2]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][NH:3]1.[H-].[Na+].[CH3:20]I>CN(C)C=O>[CH3:1][C:2]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][N:3]1[CH3:20]参加物
5
実験手順
To a solution of (+)-1-methyl-1-phenyl-1,2,3,4-tetrahydroisoquinoline (1.0 g) in N,N-dimethylformamide (10 ml) was added sodium hydride (0.19 g) in ice-bath with stirring. After stirring for 30 minutes at room temperature, to the mixture was added methyl iodide (0.31 ml). And after stirring for an hour at room temperature, the mixture was poured into ice-water and extracted with ethyl acetate. The organic layer was washed with water, sodium chloride aqueous solution, dried over magnesium sulfate and evaporated in vacuo to give (+)-1,2-dimethyl-1-phenyl-1,2,3,4-tetrahydroisoquinoline (0.6 g).
後処理
- stirringAfter stirring for 30 minutes at room temperature, to the mixture
- stirringAnd after stirring for an hour at room temperature
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water, sodium chloride aqueous solution
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-e71f606af1a64499bc7900b99c9c5d0b
- 出典データセット
- uspto-grants-1991_10
- 特許番号
- US05059608
反応ノート
読み込み中…