Ammonia → Ethyl acetate hexane

HRID 443027

반응식

HRID 443027 반응식
[OH:1][C:2]1[C:15]2[C:6](=C3C(=CN=2)C=CC=C3)[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]

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 702EthanolHCID 108623N,N-Diethyltoluene-2,5-diamine hydrochlorideHCID 22625105Phenanthridin-4-ol

생성물 1

HCID 21226206Ethyl acetate hexane수율 35.1%

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매HCID 962Water용매2회

반응 조건

온도
20 °C

실험 절차

A mixture comprising 390 mg of 4-hydroxyphenanthridine (13), 430 mg of 2-amino-5-diethylaminotoluene hydrochloride (21) and 15 ml of ethanol was stirred at 20° C. and a solution comprising 1.02 g of silver nitrate dissolved in 4.5 ml of water was added thereto drop-by-drop. Then, 1.7 ml of 25% ammonia solution was added and the 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, 259 mg of deep blue crystal of indoaniline (22) was obtained on recrystallization by hexane-ethyl acetate (yield 35.1%).

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, 259 mg of deep blue crystal of indoaniline (22)

출처 및 근거

ORD 기록
ord-4441b187230d4b449ffeb5bbcc2e61e8
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05892042

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