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Potassium Iodide → 1-pyrimidin-2-yl-1,4-diazepane

HRID 1636282
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HRID 1636282 반응식
[NH:1]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[C:9]1[N:14]=[CH:13][CH:12]=[CH:11][N:10]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>C(#N)C>[N:10]1[CH:11]=[CH:12][CH:13]=[N:14][C:9]=1[N:1]1[CH2:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 68163Hexahydro-1,4-diazepineHCID 744042-Chloropyrimidine

생성물 1

HCID 27724091-pyrimidin-2-yl-1,4-diazepane수율 48%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

50 ml of acetonitrile was added to 10.0 g (0.1 mole) of homopiperazine, 2.9 g (0.025 mole) of 2-chloropyrimidine, 6.9 g (0.05 mole) of potassium carbonate and a catalytic amount of potassium iodide, and the mixture was refluxed under heating for 11 hours. The mixture was cooled to room temperature and then filtered, the filtrate obtained was concentrated under reduced pressure, and the residue was applied to silica gel column chromatography (eluent; a chloroform:methanol=8:2 mixed solution) to obtain 2.14 g of 1-(2-pyrimidyl)homopiperazine as a pale yellow liquid.

후처리

  1. temperatureunder heating for 11 hours
  2. filtrationfiltered
  3. customthe filtrate obtained
  4. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-dd1f95b2fd884e55b18f349aa1d75c39
출처 데이터셋
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06034086

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