Ammonia → Ethyl acetate hexane

HRID 443030

反応式

HRID 443030 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.NC1C=CC(N(CC)CC)=C[C:19]=1[CH3:29].Cl.NC1C=CC(N(CC)CC)=CC=1C.N.[OH2:45]>[N+]([O-])([O-])=O.[Ag+].C(O)C>[CH3:6][CH2:15][CH2:2][CH2:3][CH2:4][CH3:5].[C:19]([O:1][CH2:2][CH3:15])(=[O:45])[CH3:29]

参加物

8

反応物 5

HCID 222AmmoniaHCID 962Water2 回HCID 673642-Amino-5-(diethylamino)tolueneHCID 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 702Ethanol溶媒

実験手順

While stirring a mixture comprising 59 mg of 4-hydroxy-6-fluorophenanthridine, 85 mg of 2-amino-5-diethylaminotoluene hydrochroride (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-f57489be2c9e4ddf9f1b244268d0d499
出典データセット
uspto-grants-1999_04
特許番号
US05892042

関連ノート

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