Dichloromethane → N-(2-Ethoxyethyl)-2-nitroaniline

HRID 1584420

反応式

HRID 1584420 の反応式
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[CH2:11]([O:13][CH2:14][CH2:15][NH2:16])[CH3:12].ClCCl>C(OCC)(=O)C>[CH2:11]([O:13][CH2:14][CH2:15][NH:16][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9])[CH3:12]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 69451-Chloro-2-nitrobenzeneHCID 66970Ethoxyethylamine

生成物 1

HCID 13623317N-(2-Ethoxyethyl)-2-nitroaniline

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

According to the method of R. Iemura et al., J. Med. Chem., 29 1178-1183 (1986), combine 1-chloro-2-nitrobenzene (69.0 g, 440 mmol) and 2-aminoethyl ethyl ether (102.5 g, 1.15 mol) and heat to reflux. After 18 hours, cool and dilute the reaction mixture with ethyl acetate (400 mL). Extract with brine. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with dichloromethane to give N-(2-ethoxyethyl)-2-nitroaniline.

後処理

  1. temperatureheat to reflux
  2. temperaturecool
  3. extractionExtract with brine
  4. dry with materialDry the organic layer over Na2SO4
  5. filtrationfilter
  6. customevaporate in vacuo
  7. customto give a residue

出典と根拠

ORDレコード
ord-67ee7f6039d041cb937549573f2775af
出典データセット
uspto-grants-1999_08
特許番号
US05932571

関連ノート

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