Piperazine → 1-[(N,N'-Di-p-tolyl)amidino]piperizine

HRID 1813885노트

반응식

HRID 1813885 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7]1([CH3:23])[CH:12]=[CH:11][C:10]([N:13]=[C:14]=[N:15][C:16]2[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=2)=[CH:9][CH:8]=1>CN(C=O)C>[C:19]1([CH3:22])[CH:20]=[CH:21][C:16]([NH:15][C:14]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)=[N:13][C:10]2[CH:9]=[CH:8][C:7]([CH3:23])=[CH:12][CH:11]=2)=[CH:17][CH:18]=1

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 69763Di-p-tolylcarbodiimide

생성물 1

HCID 99485581-[(N,N'-Di-p-tolyl)amidino]piperizine수율 52%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.2 mmol of piperazine was dissolved in 10 ml of DMF and 1.0 mmol of 1,3-di-p-tolylcarbodiimide was added. After 0.5 hour of stirring at room temperature, a small precipitation was filtered off, 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. A precipitated oil was separated by centrifugation. The residual oil was dissolved in 10 ml of methanol and 0.2 ml of conc. HCl was added. The methanol solution was concentrated to 2 ml and purified by gel filtration on Sephadex LH-20 in methanol. Yield=52%.

후처리

  1. customa small precipitation
  2. filtrationwas filtered off
  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. customA precipitated oil was separated by centrifugation
  8. dissolutionThe residual oil was dissolved in 10 ml of methanol
  9. addition0.2 ml of conc. HCl was added
  10. concentrationThe methanol solution was concentrated to 2 ml
  11. filtrationpurified by gel filtration on Sephadex

출처 및 근거

ORD 기록
ord-9d15c87cd55d4ee990477063cb17f854
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06875759B1

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