2-Aminophenol → HCID 22145448、化合物

HRID 1825282ノート

反応式

HRID 1825282 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 22145448HCID 22145448、化合物収率 81.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-ef166bc45eec4d449b71bd9ae329f07e
出典データセット
uspto-grants-2006_05
特許番号
US07045624B2

反応ノート

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