Sodium methanethiolate → 4-Sulfanylbenzene-1,3-dicarbonitrile
反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1I)[C:6]#[N:7])#[N:2].C[S-:13].[Na+]>CN(C)P(N(C)C)(N(C)C)=O>[C:1]([C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[SH:13])[C:6]#[N:7])#[N:2]参加物
4
反応条件
- 温度
- 80 °C
実験手順
Under argon, 3.03 g (12.10-3 mol) of 3-cyano-4-iodobenzonitrile and 3.36 g (48.10-3 mol) of sodium thiomethylate are dissolved in 80 ml of anhydrous hexamethylphosphoramide and the solution obtained is then heated at 80° C. for 45 minutes. The resulting reaction medium is hydrolyzed in an ice/1N HCl mixture and then extracted with methylene chloride. The organic phase is washed with water and then dried over magnesium sulfate and evaporated under reduced pressure to give 1.55 g (yield: 81%) of the expected product.
後処理
- customthe solution obtained
- customThe resulting reaction medium
- extractionextracted with methylene chloride
- washThe organic phase is washed with water
- dry with materialdried over magnesium sulfate
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-2500ab4f295340a7972ceb2a034d096d
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05246961
反応ノート
読み込み中…