Methyl iodide → HCID 53922683、化合物
反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][C:10](=[O:15])[C:11]([F:14])([F:13])[F:12])#[N:2].[H-].[Na+].[CH3:18]I>C1COCC1>[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]([CH3:18])[C:10](=[O:15])[C:11]([F:13])([F:12])[F:14])#[N:2]参加物
5
実験手順
N-(2-Cyanophenyl)-2,2,2-trifluoroacetamide (3 g, 0.014 mol) was added to sodium hydride (60% in oil, 0.62 g, 0.026 mol) in THF (40 ml) under nitrogen and stirred for 4 h. Methyl iodide (8.7 ml, 0.14 mol) was added and stirring continued overnight. The mixture was poured onto brine and extracted with ethyl acetate, dried over sodium sulphate and evaporated to give the product (3 g), MS (+EI) 228 (M+). 1H NMR (CDCl3) 7.8 (1H, d), 7.7 (1H, dd), 7.4 (1H, dd), 7.4 (1H, d), 3.43 (3H, s).
後処理
- stirringstirring continued overnight
- additionThe mixture was poured onto brine
- extractionextracted with ethyl acetate
- dry with materialdried over sodium sulphate
- customevaporated
出典と根拠
- ORDレコード
- ord-d4847f0527ba4fe6a942a99e84acd3b8
- 出典データセット
- uspto-grants-1999_03
- 特許番号
- US05883102
反応ノート
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