Ammonia → Ethyl acetate hexane

HRID 581214

반응식

HRID 581214 반응식
[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]

참가 물질

8

반응물 5

HCID 222AmmoniaHCID 962Water2회HCID 673642-Amino-5-(diethylamino)tolueneHCID 108623N,N-Diethyltoluene-2,5-diamine hydrochlorideHCID 541652404-Hydroxy-6-fluorophenanthridine

생성물 1

HCID 21226206Ethyl acetate hexane수율 27.1%

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매HCID 702Ethanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c6246c02b4f8408d9ba68288c8c28127
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05919928

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