Ammonia → Ethyl acetate hexane

HRID 482158

反応式

HRID 482158 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.Cl.NC1C=CC(N(CC)CC)=CC=1C.[CH2:30]([OH:32])[CH3:31].N>O.[N+]([O-])([O-])=O.[Ag+]>[CH3:6][CH2:15][CH2:2][CH2:3][CH2:4][CH3:5].[C:30]([O:1][CH2:2][CH3:15])(=[O:32])[CH3:31]

参加物

7

反応物 4

HCID 222AmmoniaHCID 702EthanolHCID 874624-HydroxyacridineHCID 108623N,N-Diethyltoluene-2,5-diamine hydrochloride

生成物 1

HCID 21226206Ethyl acetate hexane収率 19.6%

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 195 mg of 4-hydroxyacridine (20), 214 mg of 2-amino-5-diethylaminotoluene hydrochloride (21) and 6.8 ml of ethanol at 20° C., a solution comprising 0.17 mg of silver nitrate dissolved in 0.75 ml of water was added thereto drop-by-drop. Next, with 0.85 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, 72.5 mg of indoaniline derivative (25) described in the exemplified compound 4-1 was obtained as deep blue crystals on recrystallization by hexane-ethyl acetate (yield 19.6%).

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, 72.5 mg of indoaniline derivative (25)

出典と根拠

ORDレコード
ord-48aa29884f8f44f78ec4609ffa4d9ebc
出典データセット
uspto-grants-1998_08
特許番号
US05792863

関連ノート

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