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1,4-Diiodobutane → 2-(4-(Pyrimidin-2-ylthio)butylthio)pyrimidine

HRID 2103945
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HRID 2103945 반응식
[SH:1][C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[CH2:8](O[K])[CH3:9].I[CH2:13][CH2:14][CH2:15][CH2:16]I>C(O)C>[N:3]1[CH:4]=[CH:5][CH:6]=[N:7][C:2]=1[S:1][CH2:13][CH2:14][CH2:15][CH2:16][S:1][C:2]1[N:7]=[CH:9][CH:8]=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 123371,4-DiiodobutaneHCID 178418793HCID 178418793, 화합물HCID 178473702HCID 178473702, 화합물

생성물 1

HCID 578047232-(4-(Pyrimidin-2-ylthio)butylthio)pyrimidine수율 86%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

20 mmole of 2-mercaptopyrimidine was dissolved in 20 ml of ethanol with stirring. 20 mole of EtOK (24 weight % in ethanol) was added to the solution, stirred for 5 minutes. Then, about 10 mmole of 1,4-diiodobutane was added, and stirred overnight. The white precipitate was removed by filtration, the solvent in the filtrate was removed in vacuum. The obtained solid was dissolved in CH2Cl2, and separated with a Si gel column (solvents: 1 ethylacetate/1 hexane in volume). Yield: 86%. 1H NMR (CDCl3) of PyrC4: δ(ppm) 8.50 (4H, d, JH-H=4.77), 6.94 (2H, t, JH-H=4.77), 3.20 (4H, t, JH-H=6.93), and 1.91 (4H, t, JH-H=6.93).

후처리

  1. stirringstirred for 5 minutes
  2. stirringstirred overnight
  3. customThe white precipitate was removed by filtration
  4. customthe solvent in the filtrate was removed in vacuum
  5. dissolutionThe obtained solid was dissolved in CH2Cl2
  6. customseparated with a Si gel column (solvents: 1 ethylacetate/1 hexane in volume)

출처 및 근거

ORD 기록
ord-323fed9735a84769a9e34cba80197fb7
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07576165B2

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