Piperazine → Piperazine, 1-(phenylmethyl)-, hydrochloride (1:2)

HRID 2052806노트

반응식

HRID 2052806 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[OH-].[K+].[CH2:9]([Cl:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>[Br-].C([N+](C)(C)C)CCCCCCCCCCCCCCC.O.C1C=CC=CC=1>[ClH:16].[ClH:16].[CH2:9]([N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

7

반응물 3

HCID 4837PiperazineHCID 7503Benzyl ChlorideHCID 14797Potassium Hydroxide

생성물 1

HCID 12198046Piperazine, 1-(phenylmethyl)-, hydrochloride (1:2)수율 55%

시약·촉매·용매 3

HCID 5974Hexadecyltrimethylammonium Bromide촉매HCID 241Benzene용매HCID 962Water용매

실험 절차

A mixture of piperazine (350 mmol), KOH (100 mmol) and hexadecyl-trimethyl ammonium bromide (CTAB, 1 mmol) in water (18 ml) was heated to get a solution. Thereafter, benzyl chloride (100 mmol) in 140 ml of benzene was added to the solution dropwise at 70° C., and refluxed for 1 h. The organic layer was washed with water and saline, dried (MgSO4), filtered and evaporated, the residue was dissolved by 50 ml of ethanol and adjusted to a PH of 2 by HCl/C2H5OH (5N), the resulting precipitate was recrystallized from ethanol to obtain N-benzyl piperazine dihydrochloride (55-86%).

후처리

  1. temperaturewas heated
  2. customto get a solution
  3. temperaturerefluxed for 1 h
  4. washThe organic layer was washed with water and saline
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated
  8. dissolutionthe residue was dissolved by 50 ml of ethanol
  9. customthe resulting precipitate was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-3683190dea0e4fcfb9ee16547cfc9322
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07326710B2

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