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Hydrazine hydrate (1:1) → 3-(4-Isopropyl-piperazin-1-yl)-propylamine

HRID 325902
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반응식

HRID 325902 반응식
[CH: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)([CH3:3])[CH3:2].O.NN>C(O)C>[CH:1]([N:4]1[CH2:5][CH2:6][N:7]([CH2:10][CH2:11][CH2:12][NH2:13])[CH2:8][CH2:9]1)([CH3:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 20252235N-[3-(4-isopropyl-1-piperazinyl)propyl]phthalimide

생성물 1

HCID 128029563-(4-Isopropyl-piperazin-1-yl)-propylamine수율 59.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of N-[3-(4-isopropyl-1-piperazinyl)propyl]phthalimide (43.1 g) in ethanol (350 ml) was added 100% hydrazine hydrate (11.2 g). The resulting mixture was refluxed with stirring for 3 hours. The reaction mixture was cooled and then filtered. The filter cake was washed with ethanol. The filtrate and washing were combined and concentrated under reduced pressure. The residual oil was subjected to column chromatography (aluminum oxide), eluting with a mixture of chloroform and methanol (20:1). The fractions containing the object compound were collected and then evaporated under reduced pressure. The residual oil was distilled under reduced pressure to give 3-(4-isopropyl-1-piperazinyl)propylamine (15.0 g), (bp 45 mmHg/150° C.).

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. concentrationconcentrated under reduced pressure
  7. washeluting with a mixture of chloroform and methanol (20:1)
  8. additionThe fractions containing the object compound
  9. customwere collected
  10. customevaporated under reduced pressure
  11. distillationThe residual oil was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-2aab1a12999f4586891413b36e07e426
출처 데이터셋
uspto-grants-1984_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04443443

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