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Water → 4-(5-Nitropyridin-2-yl)piperazin-2-one

HRID 1020350
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HRID 1020350 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.C(N(CC)C(C)C)(C)C.[O:20]=[C:21]1[CH2:26][NH:25][CH2:24][CH2:23][NH:22]1.O>CN(C=O)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([N:25]2[CH2:24][CH2:23][NH:22][C:21](=[O:20])[CH2:26]2)=[N:3][CH:4]=1)([O-:10])=[O:9]
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참가 물질

6

반응물 4

HCID 962WaterHCID 783082-Chloro-5-nitropyridineHCID 81531DiisopropylethylamineHCID 231360Piperazin-2-one

생성물 1

HCID 165609144-(5-Nitropyridin-2-yl)piperazin-2-one수율 68%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매
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반응 조건

온도
85 °C

실험 절차

To a solution of 2-chloro-5-nitropyridine (623 mg, 3.9 mmol) in DMF (6 mL) was added N,N-diisopropylethylamine (1.4 mL, 8.5 mmol) and 2-oxopiperazine (424 mg, 4.24 mmol). The reaction mixture was heated at 85° C. for 40 min by microwave. Then the reaction mixture was cooled to RT, and poured into water (150 mL). The precipitate was filtered, washed with water and dried under vacuum to yield 4-(5-nitropyridin-2-yl)piperazin-2-one as a solid (588 mg, 68% yield). MS (M+1): 223.3

후처리

  1. temperatureThen the reaction mixture was cooled to RT
  2. filtrationThe precipitate was filtered
  3. washwashed with water
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-ed8316c17b304396a7b74b2786914d4c
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08716312B2

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