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Piperazine → 1-[2-(1-Methylethylamino)-3-pyrazinyl]piperazine

HRID 864392
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인쇄 미리보기

반응식

HRID 864392 반응식
Cl[C:2]1[C:7]([NH:8][CH:9]([CH3:11])[CH3:10])=[N:6][CH:5]=[CH:4][N:3]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>C1(C)C(C)=CC=CC=1.Cl>[CH3:10][CH:9]([NH:8][C:7]1[C:2]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[N:3][CH:4]=[CH:5][N:6]=1)[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 4837PiperazineHCID 214776373-Chloro-N-(propan-2-yl)pyrazin-2-amine

생성물 1

HCID 214776571-[2-(1-Methylethylamino)-3-pyrazinyl]piperazine

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 7237O-Xylene용매

실험 절차

A solution of 2-chloro-3-(1-methylethylamino)pyrazine (PREPARATION 24, 1.6 g) and piperazine (4.3 g) in xylene (10 ml) is refluxed for 26 hr. The mixture is cooled to 0o and diluted with concentrated hydrochloric acid (8 ml). The xylene is decanted and ether is added and also decanted from the salts. The salts are diluted with excess aqueous sodium hydroxide (5%) and dichloromethane. The phases are separated. The aqueous phase is extracted three more times with dichloromethane. The combined organic extracts are dried over sodium sulfate and concentrated to give a liquid mixture which is flash chromatographed on silica gel eluting with methanol/chloroform (5/95). The appropriate fractions are pooled and concentrated to give the title compound, NMR (CDCl3) 1.27, 1.83, 3.04, 4.12, 4.78, 7.49 and 7.72δ.

후처리

  1. customThe xylene is decanted
  2. additionether is added
  3. customalso decanted from the salts
  4. additionThe salts are diluted with excess aqueous sodium hydroxide (5%) and dichloromethane
  5. customThe phases are separated
  6. extractionThe aqueous phase is extracted three more times with dichloromethane
  7. dry with materialThe combined organic extracts are dried over sodium sulfate
  8. concentrationconcentrated
  9. customto give a liquid mixture which
  10. customchromatographed on silica gel eluting with methanol/chloroform (5/95)
  11. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7f6c8ed228e642e8aca1be0ffda95c44
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05563142

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