Sodium methanethiolate → 4-Sulfanylbenzene-1,3-dicarbonitrile

HRID 2372983ノート

反応式

HRID 2372983 の反応式
[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

反応物 2

HCID 4378561Sodium methanethiolateHCID 125572024-Iodoisophthalonitrile

生成物 1

HCID 147953364-Sulfanylbenzene-1,3-dicarbonitrile収率 81%

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

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

  1. customthe solution obtained
  2. customThe resulting reaction medium
  3. extractionextracted with methylene chloride
  4. washThe organic phase is washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-c7cb3ba7f96b46fa844091801d1f5ed6
出典データセット
uspto-grants-1992_03
特許番号
US05101048

反応ノート

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