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4-Bromo-2,5-dimethylbenzene-1-sulfonamide → 4-Cyano-2,5-dimethylbenzenesulfonamide

HRID 467813
ノート
印刷プレビュー

反応式

HRID 467813 の反応式
Br[C:2]1[C:7]([CH3:8])=[CH:6][C:5]([S:9]([NH2:12])(=[O:11])=[O:10])=[C:4]([CH3:13])[CH:3]=1.[Cu](C#N)[C:15]#[N:16]>CN1CCCC1=O.O1CCCC1>[C:15]([C:2]1[C:7]([CH3:8])=[CH:6][C:5]([S:9]([NH2:12])(=[O:11])=[O:10])=[C:4]([CH3:13])[CH:3]=1)#[N:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 470019584-Bromo-2,5-dimethylbenzene-1-sulfonamide2 回HCID 178418260HCID 178418260、化合物

生成物 1

HCID 666452604-Cyano-2,5-dimethylbenzenesulfonamide

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
200 °C

実験手順

To a solution of 4-bromo-2,5-dimethylbenzenesulfonamide (4.6 g, 22 mmol, the product of Step A) in N-methylpyrrolidinone (30 mL) was added copper cyanide (2.5 g, 28 mmol), and the reaction mixture was heated at 200° C. for 30 min. The reaction was then allowed to cool and poured into 200 mL of crushed ice to precipitate a solid. To this mixture was added dichloromethane (500 mL), and the mixture was warmed to dissolve the white solid. The mixture was then filtered to remove any undissolved solids, the phases were separated, and the dichloromethane was washed with water (2×100 mL), dried over magnesium sulfate, and evaporated under reduced pressure to obtain an oil. The oil was dissolved in tetrahydrofuran (30 mL) and water (30 mL), and the solution was concentrated under reduced pressure to precipitate a solid. This solid was isolated by filtration and washed with water to afford 2.5 g of the title compound. 1H NMR (CDCl3) δ 7.98 (s, 1H), 7.56 (s, 1H), 4.89 (br s, 2H), 2.66 (s, 3H), 2.58 (s, 3H).

後処理

  1. temperatureto cool
  2. customto precipitate a solid
  3. additionTo this mixture was added dichloromethane (500 mL)
  4. temperaturethe mixture was warmed
  5. dissolutionto dissolve the white solid
  6. filtrationThe mixture was then filtered
  7. customto remove any undissolved solids
  8. customthe phases were separated
  9. washthe dichloromethane was washed with water (2×100 mL)
  10. dry with materialdried over magnesium sulfate
  11. customevaporated under reduced pressure
  12. customto obtain an oil
  13. concentrationwater (30 mL), and the solution was concentrated under reduced pressure
  14. customto precipitate a solid
  15. customThis solid was isolated by filtration
  16. washwashed with water

出典と根拠

ORDレコード
ord-28778c4adc414d54b42d632684500418
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08623890B2

反応ノート

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