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Potassium Iodide → 5-(diallylamino)-1-[7-[5-(diallylamino)pentanoyl]-9H-xanthen-2-yl]pentan-1-one

HRID 1076908
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인쇄 미리보기

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HRID 1076908 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[O:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26]Cl)=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7].[I-].[K+].[CH2:31]([NH:34][CH2:35][CH:36]=[CH2:37])[CH:32]=[CH2:33]>O1CCCC1>[CH2:31]([N:34]([CH2:35][CH:36]=[CH2:37])[CH2:2][CH2:3][CH2:4][CH2:5][C:6]([C:8]1[CH:21]=[CH:20][C:19]2[O:18][C:17]3[C:12](=[CH:13][C:14]([C:22](=[O:28])[CH2:23][CH2:24][CH2:25][CH2:26][N:34]([CH2:35][CH:36]=[CH2:37])[CH2:31][CH:32]=[CH2:33])=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1)=[O:7])[CH:32]=[CH2:33]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 31279DiallylamineHCID 123402842,7-Bis(5-chlorovaleryl)-xanthene

생성물 1

HCID 5154045-(diallylamino)-1-[7-[5-(diallylamino)pentanoyl]-9H-xanthen-2-yl]pentan-1-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
120 °C

실험 절차

A mixture of 41.9 g (0.1 mole) of 2,7-bis(5-chlorovaleryl)-xanthene, 2 g of potassium iodide, 100 ml of diallylamine and 200 ml. of tetrahydrofuran was heated and stirred at 120°C. for 24 hours. After cooling, the reaction mixture was filtered and the filtrate evaporated to dryness. The resulting residue was cooled, dissolved in 10% HCl, extracted with diethyl ether and made alkaline. The product was extracted with methylene chloride, evaporated to dryness, recrystallized six times from heptane and dried in vacuo to give the desired product. M.P. 54°-55°C.

후처리

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtered
  3. customthe filtrate evaporated to dryness
  4. temperatureThe resulting residue was cooled
  5. dissolutiondissolved in 10% HCl
  6. extractionextracted with diethyl ether
  7. extractionThe product was extracted with methylene chloride
  8. customevaporated to dryness
  9. customrecrystallized six times from heptane
  10. customdried in vacuo

출처 및 근거

ORD 기록
ord-2deafccd569744edaca47e0df8d63394
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03957989

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