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Ammonia → Ethyl acetate hexane

HRID 443033
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HRID 443033 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

HCID 21226206Ethyl acetate hexane수율 12.9%

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매
HCID 962
Water
용매
2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-fd39022622144649972d930330e7c148
출처 데이터셋
uspto-grants-1999_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05892042

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