Hydrochloric Acid → Ethyl 2-(4-bromo-2-nitrophenyl)acetate

HRID 1797212노트

반응식

HRID 1797212 반응식
Cl.[CH2:2]([O:4][C:5](=[O:22])[CH:6]([C:12]1[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][C:13]=1[N+:19]([O-:21])=[O:20])C(OCC)=O)[CH3:3].O>C(O)C>[CH2:2]([O:4][C:5](=[O:22])[CH2:6][C:12]1[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][C:13]=1[N+:19]([O-:21])=[O:20])[CH3:3]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 21717185Diethyl (4-bromo-2-nitrophenyl)propanedioate

생성물 1

HCID 23247724Ethyl 2-(4-bromo-2-nitrophenyl)acetate수율 76%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred solution of concentrated HCl (18.00 mL) diluted to 72.00 mL with 95% Ethanol was added 2-(4-bromo-2-nitro-phenyl)-malonic acid diethyl ester (2.50 g, 6.94 mmol). The resulting mixture was then heated at reflux under N2 for 4 h. The reaction mixture was allowed to cool to ambient temperature and poured into H2O (250 mL). This aqueous mixture was then extracted with 2×150 mL of Diethyl ether. The Et2O layer was extracted with H2O and 5% NaHCO3 washed with brine, dried (MgSO4), and filtered. Evaporation of the filtrate in vacuo gave the intermediate title compound as a yellow liquid (1.52 g, 76%).

후처리

  1. temperatureThe resulting mixture was then heated
  2. temperatureat reflux under N2 for 4 h
  3. extractionThis aqueous mixture was then extracted with 2×150 mL of Diethyl ether
  4. extractionThe Et2O layer was extracted with H2O and 5% NaHCO3
  5. washwashed with brine
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customEvaporation of the filtrate in vacuo

출처 및 근거

ORD 기록
ord-041985fb1d65411aac1280d05aeb1246
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07034045B1

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