Potassium Cyanide → HCID 18177464、化合物

HRID 394683ノート

反応式

HRID 394683 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[O:9][CH2:8][CH:7]([CH2:13]OS(C1C=CC(C)=CC=1)(=O)=O)[CH2:6]2.[C-:25]#[N:26].[K+]>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[O:9][CH2:8][CH:7]([CH2:13][C:25]#[N:26])[CH2:6]2

参加物

4

反応物 2

HCID 9032Potassium CyanideHCID 57176004HCID 57176004、化合物

生成物 1

HCID 18177464HCID 18177464、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.6 g (4.56 mmol) of the tosylate obtained in Step B are dissolved in 25 ml of anhydrous N,N-dimethylformamide; 0.724 g (11.5 mmol) of potassium cyanide is then added to the solution. After 4 hours of reflux under argon, the solvent is evaporated in vacuo; the residue is then taken up in a saturated solution of sodium hydrogen carbonate. The aqueous phase is then extracted with dichloromethane. The organic phases, dried over magnesium sulphate and then filtered, are concentrated under reduced pressure. The title nitrile is obtained pure in the form of an oil which crystallises slowly after chromatography on silica gel (eluant: AcOEt/PE: 25/75).

後処理

  1. temperatureAfter 4 hours of reflux under argon
  2. customthe solvent is evaporated in vacuo
  3. extractionThe aqueous phase is then extracted with dichloromethane
  4. dry with materialThe organic phases, dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationare concentrated under reduced pressure

出典と根拠

ORDレコード
ord-80e5fae366fc422c96b948722490bd7d
出典データセット
uspto-grants-2003_08
特許番号
US06602903B2

反応ノート

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