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1-Nitropropane → 1-(2-Fluorophenyl)-2-nitro-1-butene

HRID 1648224
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HRID 1648224 반응식
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=O.[N+:10]([CH2:13][CH2:14][CH3:15])([O-:12])=[O:11].C([O-])(=O)C.[NH4+].C(=O)([O-])O.[Na+]>C(O)(=O)C>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[C:13]([N+:10]([O-:12])=[O:11])[CH2:14][CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 79031-NitropropaneHCID 67970o-FluorobenzaldehydeHCID 516892Sodium BicarbonateHCID 517165Ammonium Acetate

생성물 1

HCID 42261071-(2-Fluorophenyl)-2-nitro-1-butene수율 99.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

30 ml of acetic acid were added to 4.73 g (38.11 mmole) of 2-fluorobenzaldehyde, 4.41 g (49.49 mmole) of nitropropane and 3.23 g (41.90 mmole) of ammonium acetate, and the resulting mixture was heated under reflux, whilst stirring, for 4 hours. At the end of this time, the reaction mixture was cooled to room temperature, neutralized with an aqueous solution of sodium hydrogencarbonate and extracted with diethyl ether. The extract was dried over anhydrous magnesium sulfate, and then xylene was added to the solution. The mixture was concentrated by evaporation under reduced pressure, to give 7.4 g of the title compound as a pale yellow oil.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux
  3. extractionextracted with diethyl ether
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. additionxylene was added to the solution
  6. concentrationThe mixture was concentrated by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-8a20029a5bb544398c0a525a16f71cec
출처 데이터셋
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05436242

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