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

HRID 1648224
ノート
印刷プレビュー

反応式

HRID 1648224 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 42261071-(2-Fluorophenyl)-2-nitro-1-butene収率 99.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8a20029a5bb544398c0a525a16f71cec
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05436242

反応ノート

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