Sodium Carbonate → HCID 21948806、化合物

HRID 2215417ノート

反応式

HRID 2215417 の反応式
[N+:1]([C:4]1[CH:13]=[CH:12][CH:11]=[C:10]2[C:5]=1[CH:6]=[CH:7][C:8]([CH:14]=[CH2:15])=[N:9]2)([O-])=O.C(=O)([O-])[O-].[Na+].[Na+]>C(OCC)(=O)C.[Pd]>[CH2:14]([C:8]1[CH:7]=[CH:6][C:5]2[C:10](=[CH:11][CH:12]=[CH:13][C:4]=2[NH2:1])[N:9]=1)[CH3:15]

参加物

5

実験手順

1.0 g (5.0 mmol) of 5-nitro-2-vinylquinoline is dissolved in 30 ml of ethyl acetate. After 100 mg of palladium on carbon and 50 mg of sodium carbonate are added, the reaction mixture is allowed to stir for 20 hours at room temperature under hydrogen atmosphere. It is then filtered on Celite and washed with ethyl acetate. After the solvent is removed in a vacuum and after chromatography on silica gel with hexane-ethyl acetate (0–100%), then with ethyl acetate-methanol (0–30%), 720 mg (84% of theory) of the product is obtained.

後処理

  1. filtrationIt is then filtered on Celite
  2. washwashed with ethyl acetate
  3. customAfter the solvent is removed in a vacuum
  4. customafter chromatography on silica gel with hexane-ethyl acetate (0–100%), then with ethyl acetate-methanol (0–30%), 720 mg (84% of theory) of the product is obtained

出典と根拠

ORDレコード
ord-35d7c1a0c84f4481a5c1b9d8362eb24d
出典データセット
uspto-grants-2006_09
特許番号
US07109212B2

反応ノート

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