Iodoethane → 4-Bromo-1-ethoxy-2-nitrobenzene

HRID 130409

반응식

HRID 130409 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:18](I)[CH3:19]>CC(=O)CC>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:18][CH3:19])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 243644-Bromo-2-nitrophenol

생성물 1

HCID 222831884-Bromo-1-ethoxy-2-nitrobenzene

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

4-Bromo-2-nitrophenol (5.0 g, 23 mmol) and potassium carbonate (9.52 g, 69 mmol) were suspended in 2-butanone (100 ml). Ethyl iodide (2.2 ml, 28 mmol) was added dropwise at room temperature and stirred for 30 minutes. The suspension was heated at reflux for 18 hours, cooled and filtered, and the residue washed with acetone. The filtrate was concentrated in vacuo to a crude solid that was used without further purification (D14). 1H-NMR (CDCl3) δ 7.42 (1H, d, J 2.5 Hz), 7.60 (1H, dd, J 9.0, 2.5 Hz), 6.96 (1H, d, J 9.0 Hz), 4.17 (2H, q, J 7.0 Hz), 1.47 (3H, t, J 7.0 Hz).

후처리

  1. temperatureThe suspension was heated
  2. temperatureat reflux for 18 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. washthe residue washed with acetone
  6. concentrationThe filtrate was concentrated in vacuo to a crude solid that
  7. customwas used without further purification (D14)

출처 및 근거

ORD 기록
ord-fb9bc193cfa74a289e987198dbf5bdf9
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07381728B2

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