4-Methyl-3-nitrobenzoic acid → (4-Ethylpiperazin-1-yl)-(4-methyl-3-nitrophenyl)methanone

HRID 912153

반응식

HRID 912153 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=O)=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].C1C=CC2N(O)N=NC=2C=1.[CH2:24]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)[CH3:25]>ClCCl>[CH2:24]([N:26]1[CH2:31][CH2:30][N:29]([C:6]([C:5]2[CH:9]=[CH:10][C:2]([CH3:1])=[C:3]([N+:11]([O-:13])=[O:12])[CH:4]=2)=[O:8])[CH2:28][CH2:27]1)[CH3:25]

참가 물질

5

반응물 3

HCID 73194-Methyl-3-nitrobenzoic acidHCID 757711-HydroxybenzotriazoleHCID 791961-Ethylpiperazine

생성물 1

HCID 808340(4-Ethylpiperazin-1-yl)-(4-methyl-3-nitrophenyl)methanone수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To 4-methyl-3-nitro-benzoic acid (730 mg, 4.03 mmol), WSCI (930 mg, 4.85 mmol), HOBt (110 mg, 0.674 mmol) and N-ethylpiperazine (608 μl, 4.79 mmol), dichloromethane (8 ml) was added, followed by stirring for 13 hours. The reaction mixture was washed with aqueous ammonium chloride solution, and subsequently dried over sodium sulfate. After filtering sodium sulfate, the filtrate was concentrated under reduced pressure, to obtain (4-ethyl-piperazin-1-yl)-(4-methyl-3-nitro-phenyl)-methanone (1.06 g, 95%).

후처리

  1. washThe reaction mixture was washed with aqueous ammonium chloride solution
  2. dry with materialsubsequently dried over sodium sulfate
  3. filtrationAfter filtering sodium sulfate
  4. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8036c311c9f7474e8a9ec5c3ab79236f
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022205B2

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