Acetic Anhydride → HCID 21409820、化合物

HRID 2071995ノート

反応式

HRID 2071995 の反応式
[NH2:1][CH2:2][C:3]1([N:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.[C:16](OC(=O)C)(=[O:18])[CH3:17]>>[C:16]([NH:1][CH2:2][C:3]1([N:9]2[CH2:10][CH2:11][N:12]([CH3:15])[CH2:13][CH2:14]2)[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)(=[O:18])[CH3:17]

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 70181321-[1-(4-METHYLPIPERAZIN-1-YL)CYCLOHEXYL]METHANAMINE

生成物 1

HCID 21409820HCID 21409820、化合物収率 65%

実験手順

1-[1-(Aminomethyl)cyclohexyl]-4-methyl piperazine (10.57 g.,) was added slowly to stirred acetic anhydride (40 ml) cooled in ice and the stirring was continued for 15 mins. The mixture was heated under reflux for 1 hr.. The solution was evaporated to dryness and re-evaporated with ethanol/benzene (X2). The residue was dissolved in water the solution made alkaline with 5NNaOH (pH = 14), extracted with chloroform (X3), dried (anhyd.Na2SO4) and evaporated. The residue was dissolved in hot petroleum ether (80°-100° ) decolourised with charcoal and allowed to cool. The crystalline solid which formed was recrystallised from petroleum ether (b.p. 80°-100° ) to give 1-[1-(acetamidometyl)cyclohexyl]-4-methyl piperazine (8.3 g; 65%) m.p. 110°-111°.

後処理

  1. temperaturecooled in ice
  2. temperatureThe mixture was heated
  3. temperatureunder reflux for 1 hr
  4. customThe solution was evaporated to dryness
  5. customre-evaporated with ethanol/benzene (X2)
  6. dissolutionThe residue was dissolved in water the solution
  7. extractionextracted with chloroform (X3)
  8. dry with materialdried (anhyd.Na2SO4)
  9. customevaporated
  10. dissolutionThe residue was dissolved in hot petroleum ether (80°-100° )
  11. temperatureto cool
  12. customThe crystalline solid which formed
  13. customwas recrystallised from petroleum ether (b.p. 80°-100° )

出典と根拠

ORDレコード
ord-55cc1bda14c940f999678dcbbba91509
出典データセット
uspto-grants-1977_09
特許番号
US04049663

反応ノート

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