Ammonia → Ethyl acetate hexane

HRID 482156ノート

反応式

HRID 482156 の反応式
[OH:1][C:2]1[C:15]2[C:6](=C3C(=C(F)N=2)C=CC=C3)[CH:5]=[CH:4][CH:3]=1.Cl.NC1C=CC(N(CC)CC)=CC=1C.[CH2:31]([OH:33])[CH3:32].N>O.[N+]([O-])([O-])=O.[Ag+]>[CH3:6][CH2:15][CH2:2][CH2:3][CH2:4][CH3:5].[C:31]([O:1][CH2:2][CH3:15])(=[O:33])[CH3:32]

参加物

7

反応物 4

HCID 222AmmoniaHCID 702EthanolHCID 108623N,N-Diethyltoluene-2,5-diamine hydrochlorideHCID 541652404-Hydroxy-6-fluorophenanthridine

生成物 1

HCID 21226206Ethyl acetate hexane収率 27.1%

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 59 mg of 4-hydroxy-6-fluorophenanthridine, 85 mg of 2-amino-5-diethylaminotoluene hydrochloride (21) and 4 ml of ethanol at 20° C., a solution comprising 258 mg of silver nitrate dissolved in 0.8 ml of water was added thereto drop-by-drop. Next, with 0.84 ml of 25% ammonia solution added, 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 chloroform, the extract was concentrated. After purification by column chromatography, 29 mg of indoaniline described in the exemplified compound 3-131 was obtained as deep blue crystal on recrystallization from hexane-ethyl acetate solvent (yield 27.1%).

後処理

  1. additionwas added
  2. customreaction
  3. customAfter the completion of the reaction
  4. extractionAfter extraction by chloroform
  5. concentrationthe extract was concentrated
  6. customAfter purification by column chromatography, 29 mg of indoaniline

出典と根拠

ORDレコード
ord-820e4df88a584121984737ce2f3c5bd7
出典データセット
uspto-grants-1998_08
特許番号
US05792863

反応ノート

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