Ammonia → Ethyl acetate hexane

HRID 581217

反応式

HRID 581217 の反応式
[OH:1][C:2]1[C:15]2[C:6](=CC3C(N=2)=CC=CC=3)[CH:5]=[CH:4][CH:3]=1.C(C(CCCC)CN(CC(CC)CCCC)C1C=CC(N)=CC=1)C.[CH2:40]([OH:42])[CH3:41].N>O.[N+]([O-])([O-])=O.[Ag+]>[CH3:6][CH2:15][CH2:2][CH2:3][CH2:4][CH3:5].[C:40]([O:1][CH2:2][CH3:15])(=[O:42])[CH3:41]

参加物

7

反応物 4

HCID 222AmmoniaHCID 702EthanolHCID 874624-HydroxyacridineHCID 53999179n,n-Di(2-ethylhexyl)-p-phenylenediamine

生成物 1

HCID 21226206Ethyl acetate hexane収率 12.9%

試薬・触媒・溶媒 2

HCID 24470Silver Nitrate触媒HCID 962Water溶媒2 回

実験手順

While stirring a mixture comprising 2.87 g of 4-hydroxyacridine (20), 4.89 g of N,N-di(2-ethylhexyl)-p-phenylenediamine and 100 ml of ethanol at 20° C., a solution comprising 7.48 g of silver nitrate dissolved in 33.1 ml of water was added thereto drop-by-drop. Next, with 12.5 ml of 25% ammonia solution added to the mixture, reaction was allowed to proceed at 20° C. for a period of 24 hr. After the completion of the reaction, the reacted solution was introduced into water. After extraction by ethyl acetate, the extract was concentrated. After purification by column chromatography, 0.99 g of indoaniline described in the exemplified compound 4-10 was obtained as deep blue crystals on recrystallization by hexane-ethyl acetate (yield 12.9%).

後処理

  1. additionwas added
  2. customAfter the completion of the reaction
  3. extractionAfter extraction by ethyl acetate
  4. concentrationthe extract was concentrated
  5. customAfter purification by column chromatography, 0.99 g of indoaniline

出典と根拠

ORDレコード
ord-1442a3f3f77543eeb091c6988b8d7ede
出典データセット
uspto-grants-1999_07
特許番号
US05919928

関連ノート

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