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2-Benzylpyrazine → 2-Benzylpiperazine

HRID 344901
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HRID 344901 반응식
[CH2:1]([C:8]1[CH:13]=[N:12][CH:11]=[CH:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)(=O)C.[Pt](=O)=O>[CH2:1]([CH:8]1[CH2:13][NH:12][CH2:11][CH2:10][NH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 5203702-Benzylpyrazine

생성물 1

HCID 5590332-Benzylpiperazine수율 64.2%

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 176Acetic Acid용매

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온도
20 °C

실험 절차

A solution of 2-benzylpyrazine (8 g) in acetic acid (60 cc) is treated with platinum dioxide (0.8 g) and hydrogenated under a pressure of 1 atmosphere at approximately 20° C. When the absorption of hydrogen is complete, the catalyst is removed by filtration through diatomaceous silica. The solution is concentrated to dryness under reduced pressure (20 kPa) at approximately 60° C. The dry extract is suspended in ethanol (40 cc) and treated at approximately 20° C. with a solution of sodium ethylate prepared from sodium (1.49 g) in ethanol (40 cc). After 2 hours' stirring at approximately 20° C., the suspension is concentrated to dryness under reduced pressure (20 kPa) at approximately 30° C. The dry extract is taken up with ethyl ether (60 cc). The insoluble matter is removed by filtration through diatomaceous silica. The filtrate is concentrated to dryness under reduced pressure under the same conditions as above. The dry extract is taken up with isopropyl ether (20 cc), drained and washed with the same solvent (2×5 cc). (RS)-2-Benzylpiperazine (5.32 g) is obtained in the form of a light beige solid, m.p. 90° C.

후처리

  1. customWhen the absorption of hydrogen
  2. customthe catalyst is removed by filtration through diatomaceous silica
  3. concentrationThe solution is concentrated to dryness under reduced pressure (20 kPa) at approximately 60° C
  4. extractionThe dry extract
  5. additiontreated at approximately 20° C. with a solution of sodium ethylate
  6. customprepared from sodium (1.49 g) in ethanol (40 cc)
  7. concentrationthe suspension is concentrated to dryness under reduced pressure (20 kPa) at approximately 30° C
  8. extractionThe dry extract
  9. customThe insoluble matter is removed by filtration through diatomaceous silica
  10. concentrationThe filtrate is concentrated to dryness under reduced pressure under the same conditions as above
  11. extractionThe dry extract
  12. washwashed with the same solvent (2×5 cc)

출처 및 근거

ORD 기록
ord-e8955fce54b2478a958998f1ac2765a1
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05053509

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