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2-Benzylpyrazine → 2-Benzylpiperazine

HRID 344901
ノート
印刷プレビュー

反応式

HRID 344901 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 5203702-Benzylpyrazine

生成物 1

HCID 5590332-Benzylpiperazine収率 64.2%

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 176Acetic Acid溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e8955fce54b2478a958998f1ac2765a1
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05053509

反応ノート

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