HCID 22013736、化合物 → HCID 22013776、化合物

HRID 1532690ノート

反応式

HRID 1532690 の反応式
[CH3:1][N:2]([CH3:19])[CH2:3][CH2:4][NH:5][C:6]1[CH:15]=[CH:14][C:9]([C:10]([NH:12][CH3:13])=[O:11])=[CH:8][C:7]=1[N+:16]([O-])=O>C(OCC)(=O)C.C(O)C.[C].[Pd]>[NH2:16][C:7]1[CH:8]=[C:9]([CH:14]=[CH:15][C:6]=1[NH:5][CH2:4][CH2:3][N:2]([CH3:1])[CH3:19])[C:10]([NH:12][CH3:13])=[O:11]

参加物

5

反応物 1

HCID 22013736HCID 22013736、化合物

生成物 1

HCID 22013776HCID 22013776、化合物収率 87.7%

試薬・触媒・溶媒 3

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

10% of palladium-carbon (0.738 g) was added to a solution containing 4-{[2-(dimethylamino)ethyl]amino}-N-methyl-3-nitrobenzamide (3.679 g) in a mixture of ethyl acetate (40 ml) and ethanol (37 ml), and the mixture was stirred for 4.5 hours under a hydrogen gas atmosphere at room temperature. After the catalyst was removed out by filtration, the filtrate was concentrated. The residue, with ethyl acetate added thereto, was washed with 1N sodium hydroxide aqueous solution and saturated brine successively, dried over sodium sulfate anhydride, and concentrated, thereby yielding the entitled compound (2.862 g) as brown solid.

後処理

  1. customAfter the catalyst was removed out by filtration
  2. concentrationthe filtrate was concentrated
  3. additionThe residue, with ethyl acetate added
  4. washwas washed with 1N sodium hydroxide aqueous solution and saturated brine successively
  5. dry with materialdried over sodium sulfate anhydride
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-266c1b073c7041498535b829c453d6cb
出典データセット
uspto-grants-2001_03
特許番号
US06204264B1

反応ノート

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