2-Aminophenol → HCID 22145448, 화합물

HRID 1825282노트

반응식

HRID 1825282 반응식
Cl.CN([CH:5]([CH3:15])[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=1)=[O:7])C.[NH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[OH:23]>C(O)C>[ClH:14].[OH:23][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[NH:16][CH2:15][CH2:5][C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=1)=[O:7]

참가 물질

4

반응물 2

HCID 58012-AminophenolHCID 695907691-(3-Chlorophenyl)-2-(dimethylamino)propan-1-one hydrochloride (1:1)

생성물 1

HCID 22145448HCID 22145448, 화합물수율 81.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Dimethylamino-m-chloropropiophenone hydrochloride (74.9 g, 0.30 mol) was dissolved in 50% aqueous ethanol (700 ml) at reflux. 2-Aminophenol (32.9 g, 0.30 mol) was then added and the resulting red solution was refluxed for a further 2 hours. The reaction mixture was allowed to cool to room temperature and then extracted twice with ethyl acetate (2×100 ml). Note that brine was also added at this point to allow the two layers to separate effectively). The organic extracts were combined and an excess of concentrated hydrochloric acid (47 ml) was added. The solution was concentrated in vacuo and then allowed to cool. The precipitate that formed was filtered of, washed with diethyl ether and dried in vacuo to yield a cream powder (38.1 g, 40%).

후처리

  1. temperatureat reflux
  2. temperaturethe resulting red solution was refluxed for a further 2 hours
  3. extractionextracted twice with ethyl acetate (2×100 ml)
  4. additionwas also added at this point
  5. customto separate effectively)
  6. additionan excess of concentrated hydrochloric acid (47 ml) was added
  7. concentrationThe solution was concentrated in vacuo
  8. temperatureto cool
  9. customThe precipitate that formed
  10. filtrationwas filtered of,
  11. washwashed with diethyl ether
  12. customdried in vacuo

출처 및 근거

ORD 기록
ord-ef166bc45eec4d449b71bd9ae329f07e
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07045624B2

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