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1-Methylpiperazine → 1-[(N,N'-Di-p-tolyl)amidino]-4-methyl-piperizine

HRID 1813884
ノート
印刷プレビュー

反応式

HRID 1813884 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[C:8]1([CH3:24])[CH:13]=[CH:12][C:11]([N:14]=[C:15]=[N:16][C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][CH:18]=2)=[CH:10][CH:9]=1>CN(C=O)C>[C:8]1([CH3:24])[CH:13]=[CH:12][C:11]([NH:14][C:15]([N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)=[N:16][C:17]2[CH:18]=[CH:19][C:20]([CH3:23])=[CH:21][CH:22]=2)=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 69763Di-p-tolylcarbodiimide

生成物 1

HCID 98836421-[(N,N'-Di-p-tolyl)amidino]-4-methyl-piperizine収率 78%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.05 mmol of 1-methylpiperazine was dissolved in 10 ml of N,N′-dimethylformamide (DMF), and 1.0 mmol of 1,3-di-p-tolylcarbodiimide was added. After 0.5 h. of stirring at room temperature, a small precipitation was removed by filtration and washed twice with 1 ml of DMF. The filtrates were collected and kept at room temperature overnight. 50 ml of water was added to the solution. An oil precipitated after 0.5 h which transformed into a solid. The solid residue was collected by filtration, washed twice with water and dissolved in 20 ml of methanol. 0.2 ml of conc. HCl was added was added to the methanol solution. After evaporation of the methanol, the residue was redissolved in methanol, and pure product was precipitated from the solution with ethyl ether. Yield=78%.

後処理

  1. customa small precipitation
  2. customwas removed by filtration
  3. washwashed twice with 1 ml of DMF
  4. customThe filtrates were collected
  5. waitkept at room temperature overnight
  6. addition50 ml of water was added to the solution
  7. customAn oil precipitated after 0.5 h which
  8. filtrationThe solid residue was collected by filtration
  9. washwashed twice with water
  10. dissolutiondissolved in 20 ml of methanol
  11. addition0.2 ml of conc. HCl was added
  12. additionwas added to the methanol solution
  13. customAfter evaporation of the methanol
  14. dissolutionthe residue was redissolved in methanol
  15. custompure product was precipitated from the solution with ethyl ether

出典と根拠

ORDレコード
ord-9d916d402986456aaad4ee4eb054c539
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06875759B1

反応ノート

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