4-Aminophenol → 4-[3-(t-Butylamino)-2-hydroxypropoxy]aniline

HRID 328906노트

반응식

HRID 328906 반응식
[CH:1]1[C:6]([NH2:7])=[CH:5][CH:4]=[C:3]([OH:8])[CH:2]=1.[C:9]([N:13]1[CH2:16][CH:15]([OH:17])[CH2:14]1)([CH3:12])([CH3:11])[CH3:10].[OH-].[K+]>Cl>[NH2:7][C:6]1[CH:5]=[CH:4][C:3]([O:8][CH2:16][CH:15]([OH:17])[CH2:14][NH:13][C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:2][CH:1]=1

참가 물질

5

반응물 3

HCID 4034-AminophenolHCID 14797Potassium HydroxideHCID 2879861-tert-Butyl-3-hydroxyazetidine

생성물 1

HCID 126663354-[3-(t-Butylamino)-2-hydroxypropoxy]aniline

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
140 °C

실험 절차

A mixture of 21.8 g of p-aminophenol, 22 g of 1-(tert.-butyl)-3-azetidinol and 0.73 g of potassium hydroxide was heated under nitrogen gas at 140° C. for 8 hours with agitation. The reaction mixture was cooled and dissolved in concentrated hydrochloric acid and the solution was extracted with ether. The hydrochloric acid aqueous solution was made alkaline with 10% -NaOH aqueous solution and then extracted with ether. The ether solution was washed with water and dried over anhydrous sodium sulfate. Then ether was distilled off and the residue was recrystallized from benzene. As a result 8g of 1-(p-aminophenoxy)-3-(tert.-butylamino)-2-propanol melting at 125° - 127° C were obtained. The results of infra-red spectrum analysis and nuclear magnetic resonance analysis are as follows:

후처리

  1. temperatureThe reaction mixture was cooled
  2. extractionthe solution was extracted with ether
  3. extractionextracted with ether
  4. washThe ether solution was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThen ether was distilled off
  7. customthe residue was recrystallized from benzene

출처 및 근거

ORD 기록
ord-d1149e37528d4083bfd8b622e5646aee
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018824

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