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Potassium Iodide → HCID 19909642, 화합물

HRID 1534357
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HRID 1534357 반응식
N1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7]CCCl.[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.[I-].[K+].[CH3:25][N:26]([CH3:29])C=O>>[N:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[N:17]1[CH2:18][CH2:19][N:20]([CH2:6][CH2:5][CH2:4][C:3]2[CH:25]=[N:26][CH:29]=[CH:7][CH:2]=2)[CH2:21][CH2:22]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 4875Potassium IodideHCID 6228DimethylformamideHCID 944591-(2-Pyridyl)piperazineHCID 1791132-(3-Chloro-propyl)-pyridine

생성물 1

HCID 19909642HCID 19909642, 화합물

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온도
80 °C

실험 절차

A solution of 3-pyridinylpropylchloride (Example A) (3.0 g, 0.0193 mol), 1-(2-pyridinyl)piperazine (3.15 g, 0.0193 mol), potassium iodide (0.8 g, 0.005 mol) is dissolved in N,N-dimethylformamide (80 mL) and heated to 80° C. for 12 hours. The reaction is cooled and the precipitate is filtered. The filtrate is washed with sodium carbonate and extracted with dichloromethane. The organic layer is evaporated in vacuo and the residue is purified by column chromatography (silica gel, 10% ethanol/ethyl acetate). The major product is taken up in diethyl ether and the precipitate is filtered. The filtrate is evaporated in vacuo to give 0.8 g of 1-(2-pyridinyl)-4-[3-(3-pyridinyl)propyl]piperazine as a white solid; mp 51-52° C.

후처리

  1. temperatureThe reaction is cooled
  2. filtrationthe precipitate is filtered
  3. washThe filtrate is washed with sodium carbonate
  4. extractionextracted with dichloromethane
  5. customThe organic layer is evaporated in vacuo
  6. customthe residue is purified by column chromatography (silica gel, 10% ethanol/ethyl acetate)
  7. filtrationthe precipitate is filtered
  8. customThe filtrate is evaporated in vacuo

출처 및 근거

ORD 기록
ord-53641a4cb697449b885deb709e573bca
출처 데이터셋
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05089497

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