1-Chloro-2-nitrobenzene → N-(2-Ethoxyethyl)-2-nitroaniline

HRID 746210

반응식

HRID 746210 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1Cl)([O-:3])=[O:2].[CH2:11]([O:13][CH2:14][CH2:15][NH2:16])[CH3:12]>C(OCC)(=O)C>[CH2:11]([O:13][CH2:14][CH2:15][NH:16][C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[N+:1]([O-:3])=[O:2])[CH3:12]

참가 물질

4

반응물 2

HCID 69451-Chloro-2-nitrobenzeneHCID 66970Ethoxyethylamine

생성물 1

HCID 13623317N-(2-Ethoxyethyl)-2-nitroaniline수율 107.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
130 °C

실험 절차

A mixture of o-nitrochlorobenzene (30 g) and 2-ethoxyethylamine (51 g) is stirred at 130° C. for 3 hours. After allowing to cool, ethyl acetate (150 ml) is added to the reaction mixture, and the ethyl acetate layer is separated, washed three times with saturated aqueous saline, dried over anhydrous magnesium sulfate, and then concentrated. The residue is distilled under reduced pressure to give N-(2-ethoxyethyl)-o-nitroaniline (42.9 g) as a reddish brown liquid, b.p. 144°-145.5° C./1.0 mmHg.

후처리

  1. temperatureto cool
  2. customthe ethyl acetate layer is separated
  3. washwashed three times with saturated aqueous saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. distillationThe residue is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-48e43cbef703412dbb45dc5e8243e257
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04603130

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