Sodium Acetate → HCID 18177433、化合物

HRID 394684ノート

反応式

HRID 394684 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][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

参加物

7

反応物 3

HCID 517045Sodium AcetateHCID 18177464HCID 18177464、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 18177433HCID 18177433、化合物

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 7918Acetic Anhydride溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8c74c5a2c50341ae9a37020018a12e74
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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