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Hydrazine hydrate (1:1) → 3-[4-(Prop-2-EN-1-YL)piperazin-1-YL]propan-1-amine

HRID 1284620
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반응식

HRID 1284620 반응식
[CH2:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][CH2:12][N:13]2C(=O)C3=CC=CC=C3C2=O)[CH2:6][CH2:5]1)[CH:2]=[CH2:3].O.NN>C(O)C>[CH2:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][CH2:12][NH2:13])[CH2:6][CH2:5]1)[CH:2]=[CH2:3]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 20252233HCID 20252233, 화합물

생성물 1

HCID 202522303-[4-(Prop-2-EN-1-YL)piperazin-1-YL]propan-1-amine수율 90.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of N-[3-(4-allyl-1-piperazinyl)propyl]phthalimide (35.6 g) in ethanol (400 ml) was added 100% hydrazine hydrate (14.3 g). The resulting mixture was refluxed with stirring for 2.5 hours. The reaction mixture was cooled and then filtered. The filter cake was washed with ethanol. The filtrate and washing were combined and evaporated under reduced pressure. The residual oil was subjected to column chromatigraphy (aluminum oxide), eluting with a mixture of chloroform and methanol (10:1). The fractions containing the object compound were collected and then evaporated under reduced pressure to give an oil of 3-(4-allyl-1-piperazinyl)propylamine (18.8 g).

후처리

  1. temperatureThe resulting mixture was refluxed
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. washThe filter cake was washed with ethanol
  5. washThe filtrate and washing
  6. customevaporated under reduced pressure
  7. washeluting with a mixture of chloroform and methanol (10:1)
  8. additionThe fractions containing the object compound
  9. customwere collected
  10. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-015194ee3f7e4bb2a1ee20e2dedd116d
출처 데이터셋
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04563524

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