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Hydrogen iodide → 2-hexylthio-7-iodo-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one

HRID 1073790
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HRID 1073790 반응식
Cl[C:2]1[N:3]=[C:4]2[S:11][C:10]([S:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[N:9][N:5]2[C:6](=[O:8])[CH:7]=1.[IH:19]>>[I:19][C:2]1[N:3]=[C:4]2[S:11][C:10]([S:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18])=[N:9][N:5]2[C:6](=[O:8])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 24841Hydrogen iodideHCID 156107907-chloro-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one

생성물 1

HCID 156107912-hexylthio-7-iodo-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one수율 80%

실험 절차

A solution of 8.4 g of the thus obtained 7-chloro-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]-pyrimidin-5-one and 88.2 g of a 57% hydroiodic acid aqueous solution was heated to 95°~110° C. and stirred for 2 hours. After cooling, the solution was filtered. The residue was washed with water and dissolved in toluene. The toluene solution was washed with a sodium hydrogen carbonate aqueous solution, a sodium thiosulfate aqueous solution and water respectively and dried over anhydrous sodium sulfate. The solvent was distilled off and thus 9.8 g of 80% pure 7-iodo-2-hexylthio-5H-1,3,4-thiadiazolo[3,2-a]pyrimidin-5-one was obtained. Yield 72%.

후처리

temperature
After cooling
  • filtrationthe solution was filtered
  • washThe residue was washed with water
  • dissolutiondissolved in toluene
  • washThe toluene solution was washed with a sodium hydrogen carbonate aqueous solution
  • dry with materiala sodium thiosulfate aqueous solution and water respectively and dried over anhydrous sodium sulfate
  • distillationThe solvent was distilled off
  • 출처 및 근거

    ORD 기록
    ord-61452dcbde6d4c72b8beffc7c8f175de
    출처 데이터셋
    uspto-grants-1990_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04971971

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