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tert-Butyl piperazine-1-carboxylate → Tert-butyl 4-(3-nitropyridin-4-yl)piperazine-1-carboxylate

HRID 2066613
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HRID 2066613 반응식
[N+:1]([C:4]1[CH:5]=[N:6][CH:7]=[CH:8][C:9]=1Cl)([O-:3])=[O:2].C(N(CC)C(C)C)C.[C:19]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20]>ClCCl>[C:22]([O:21][C:19]([N:26]1[CH2:31][CH2:30][N:29]([C:9]2[CH:8]=[CH:7][N:6]=[CH:5][C:4]=2[N+:1]([O-:3])=[O:2])[CH2:28][CH2:27]1)=[O:20])([CH3:25])([CH3:23])[CH3:24]
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참가 물질

5

반응물 3

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 521913N,N-Diethyl-2-propanamineHCID 27357814-Chloro-3-nitropyridine

생성물 1

HCID 59332343Tert-butyl 4-(3-nitropyridin-4-yl)piperazine-1-carboxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

3-Nitro-4-Chloro pyridine (10 mmol) dissolved in dichloromethane (25 mL) and diethyl iso propyl amine (20 mmol) followed Boc piperazine(10 mmol) was added to the above solution while cooling at 0° C. and the reaction mixture was stirred at room temperature for overnight . The dichloromethane was evaporated under vacuum. The resulting solid is extracted in to dichloromethane and washed with citric acid and brine solution. The evaporation of dichloromethane gave a yellow solid, 4-(3-Nitro-pyridin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester which is used for next step without purification.

후처리

  1. additionwas added to the above solution
  2. customThe dichloromethane was evaporated under vacuum
  3. extractionThe resulting solid is extracted in to dichloromethane
  4. washwashed with citric acid and brine solution
  5. customThe evaporation of dichloromethane

출처 및 근거

ORD 기록
ord-995d34cb4cd3417ca37b0837391ee486
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08293747B2

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