Potassium Cyanide → HCID 18177464, 화합물

HRID 394683노트

반응식

HRID 394683 반응식
[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

참가 물질

4

반응물 2

HCID 9032Potassium CyanideHCID 57176004HCID 57176004, 화합물

생성물 1

HCID 18177464HCID 18177464, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-80e5fae366fc422c96b948722490bd7d
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06602903B2

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