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Hydrazine → HCID 13035121, 화합물

HRID 1075396
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HRID 1075396 반응식
Cl.Cl[CH2:3][CH2:4][CH2:5][N:6]1[CH2:11][CH2:10][N:9]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[CH:13]=2)[CH2:8][CH2:7]1.[NH2:19][NH2:20]>C(O)(C)C>[Cl:18][C:14]1[CH:13]=[C:12]([N:9]2[CH2:10][CH2:11][N:6]([CH2:5][CH2:4][CH2:3][NH:19][NH2:20])[CH2:7][CH2:8]2)[CH:17]=[CH:16][CH:15]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 130351201-(3-Chlorophenyl)-4-(3-chloropropyl)piperazinium chloride

생성물 1

HCID 13035121HCID 13035121, 화합물수율 94.5%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
75 °C

실험 절차

1-(3-Chloropropyl)-4-(3-chlorophenyl)piperazine hydrochloride (20.0 g, 0.065 mol) is suspended in isopropanol (65 ml) and anhydrous hydrazine (31.7 g, 0.988 mol) is added. The reaction mixture is heated at 70-80° C. for 2.5 hours and cooled to room temperature. The upper layer is separated and concentrated under reduced pressure. The residue is dissolved in isopropanol (50 ml) and the upper layer is separated, dried (Na2SO4), and concentrated to yield 16.5 g (94.5% yield) of 1-(3-chlorophenyl)-4-(3-hydrazinopropyl)piperazine (85% pure) as a viscous oil. The product is used directly without further purification or stored at room temperature in toluene or isopropanol solution by adding 1% MgO.

후처리

  1. temperaturecooled to room temperature
  2. customThe upper layer is separated
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue is dissolved in isopropanol (50 ml)
  5. customthe upper layer is separated
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8cd220b50413401ca8d489a506dfe3fe
출처 데이터셋
uspto-grants-1999_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05900485

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