cis-3,5-Dimethyl-1-[4-(methyloxy)-3-nitrophenyl]piperazine → 5-(cis-3,5-Dimethyl-1-piperazinyl)-2-(methyloxy)aniline

HRID 130400노트

반응식

HRID 130400 반응식
[CH3:1][C@H:2]1[NH:7][C@@H:6]([CH3:8])[CH2:5][N:4]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[C:11]([N+:17]([O-])=O)[CH:10]=2)[CH2:3]1>C(O)C.[Pd]>[CH3:8][C@H:6]1[NH:7][C@@H:2]([CH3:1])[CH2:3][N:4]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[C:11]([CH:10]=2)[NH2:17])[CH2:5]1

참가 물질

4

반응물 1

HCID 59007052cis-3,5-Dimethyl-1-[4-(methyloxy)-3-nitrophenyl]piperazine

생성물 1

HCID 590070635-(cis-3,5-Dimethyl-1-piperazinyl)-2-(methyloxy)aniline

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A mixture of cis-3,5-dimethyl-1-[4-(methyloxy)-3-nitrophenyl]piperazine (D3) (2.65 g, 10 mmol) in ethanol (60 ml) containing palladium on charcoal (300 mg, 10% paste) was stirred under aone atmosphere of hydrogen gas overnight. The mixture was filtered through celite, the pad washed in ethanol and the combined ethanol solutions evaporated. The residue was purified by column chromatography (Biotage (SiO2) 100 g, dichloromethane to 1:10 2M ammonia in methanol:dichloromethane) to afford the title product (D4). MS (ES+) m/e 236 [M+H]+.

후처리

  1. filtrationThe mixture was filtered through celite
  2. washthe pad washed in ethanol
  3. customthe combined ethanol solutions evaporated
  4. customThe residue was purified by column chromatography (Biotage (SiO2) 100 g, dichloromethane to 1:10 2M ammonia in methanol:dichloromethane)

출처 및 근거

ORD 기록
ord-02667bc13b9349a1a9663f31c9975be8
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07381728B2

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