HCID 22013736, 화합물 → HCID 22013776, 화합물

HRID 1532690노트

반응식

HRID 1532690 반응식
[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]

참가 물질

5

반응물 1

HCID 22013736HCID 22013736, 화합물

생성물 1

HCID 22013776HCID 22013776, 화합물수율 87.7%

시약·촉매·용매 3

HCID 178418390HCID 178418390, 화합물촉매HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-266c1b073c7041498535b829c453d6cb
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06204264B1

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