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Nitroethane → 2,4-Dichloro-1-(2-nitro-1-propen-1-yl)benzene

HRID 389171
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반응식

HRID 389171 반응식
[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH:4]=O.C([O-])(=O)C.[NH4+].[N+:16]([CH2:19][CH3:20])([O-:18])=[O:17]>C(OCC)(=O)C>[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH:4]=[C:19]([N+:16]([O-:18])=[O:17])[CH3:20]
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참가 물질

5

반응물 3

HCID 6587NitroethaneHCID 134042,4-DichlorobenzaldehydeHCID 517165Ammonium Acetate

생성물 1

HCID 7106762,4-Dichloro-1-(2-nitro-1-propen-1-yl)benzene수율 52%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 2,4-dichlorobenzaldehyde (1.45 g, 8.3 mmol), ammonium acetate (0.64 g, 8.3 mmol) and nitroethane (6 g, 80 mmol) was heated under reflux for 6 hr. The mixture was allowed to cool to room temperature and ethyl acetate was added. The mixture was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated. Recrystallization from ethanol gave 2,4-dichloro-1-(2-nitro-1-propenyl)benzene (yellow needle crystals, yield; 1.0 g, 52%).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hr
  3. washThe mixture was washed with water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customRecrystallization from ethanol

출처 및 근거

ORD 기록
ord-1399554a04494fd9a666bf997f38615d
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08378114B2

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