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

HRID 6019

반응식

HRID 6019 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

반응 조건

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-2500ab4f295340a7972ceb2a034d096d
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05246961

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