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

HRID 1076908
ノート
印刷プレビュー

反応式

HRID 1076908 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2deafccd569744edaca47e0df8d63394
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03957989

反応ノート

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