Sodium Acetate → HCID 18177433, 화합물

HRID 394684노트

반응식

HRID 394684 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][C:14]#[N:15])[CH2:6]2.[C:16]([O-])(=[O:18])[CH3:17].[Na+].[H][H]>[Ni].C(OC(=O)C)(=O)C.C(OCC)(=O)C>[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][CH2:14][NH:15][C:16](=[O:18])[CH3:17])[CH2:6]2

참가 물질

7

반응물 3

HCID 517045Sodium AcetateHCID 18177464HCID 18177464, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 18177433HCID 18177433, 화합물

시약·촉매·용매 3

HCID 935Nickel촉매HCID 7918Acetic Anhydride용매HCID 8857Ethyl Acetate용매

실험 절차

0.812 g (4 mmol) of the nitrile obtained in Step C is added to a suspension of 0.35 g (6 mmol) of Raney nickel and 0.5 g (6 mmol) of sodium acetate in 40 ml of acetic anhydride. The reaction medium is then subjected to hydrogen pressure of 50 psi at a temperature of 50° C. for 5 hours. After cooling of the mixture, the salts are filtered off and the filtrate is concentrated under reduced pressure. The residue obtained is then taken up in ethyl acetate; the organic phase is then washed with a saturated solution of sodium hydrogen carbonate. After drying over magnesium sulphate and filtration, the solvent is evaporated in vacuo. Chromatography on a silica column (eluant: AcOEt) results in the title amide in the form of a white solid.

후처리

  1. temperatureAfter cooling of the mixture
  2. filtrationthe salts are filtered off
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customThe residue obtained
  5. washthe organic phase is then washed with a saturated solution of sodium hydrogen carbonate
  6. dry with materialAfter drying over magnesium sulphate and filtration
  7. customthe solvent is evaporated in vacuo

출처 및 근거

ORD 기록
ord-8c74c5a2c50341ae9a37020018a12e74
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06602903B2

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