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

HRID 2372983노트

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HRID 2372983 반응식
[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]

참가 물질

4

반응물 2

HCID 4378561Sodium methanethiolateHCID 125572024-Iodoisophthalonitrile

생성물 1

HCID 147953364-Sulfanylbenzene-1,3-dicarbonitrile수율 81%

시약·촉매·용매 1

HCID 12679Hexamethylphosphoramide용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c7cb3ba7f96b46fa844091801d1f5ed6
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05101048

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