Water → 1-Fluoro-3-((E)-2-nitro-vinyl)-5-propoxy-benzene

HRID 20437ノート

反応式

HRID 20437 の反応式
C([O-])(=O)C.[NH4+].[F:6][C:7]1[CH:8]=[C:9]([CH:12]=[C:13]([O:15][CH2:16][CH2:17][CH3:18])[CH:14]=1)[CH:10]=O.[N+:19]([CH3:22])([O-:21])=[O:20].O>C(O)(=O)C>[F:6][C:7]1[CH:14]=[C:13]([O:15][CH2:16][CH2:17][CH3:18])[CH:12]=[C:9](/[CH:10]=[CH:22]/[N+:19]([O-:21])=[O:20])[CH:8]=1

参加物

6

反応物 4

HCID 962WaterHCID 6375NitromethaneHCID 517165Ammonium AcetateHCID 862368003-Fluoro-5-propoxybenzaldehyde

生成物 1

HCID 685582311-Fluoro-3-((E)-2-nitro-vinyl)-5-propoxy-benzene収率 69.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
140 °C

実験手順

Add ammonium acetate (2.63 g, 34.08 mmol) to 3-fluoro-5-propoxy-benzaldehyde (2.25 g, 12.35 mmol) and nitromethane (3.09 g, 50.63 mmol) in acetic acid (41 mL) at room temperature and heat in 140° C. oil bath for 3 hours. Cool to room temperature and pour into water. Extract with ethyl acetate, dry over magnesium sulfate, filter and concentrate to afford 1.94 g (69.8%) of the desired compound as an oil.

後処理

  1. temperatureCool to room temperature
  2. extractionExtract with ethyl acetate
  3. dry with materialdry over magnesium sulfate
  4. filtrationfilter
  5. concentrationconcentrate

出典と根拠

ORDレコード
ord-a207859cfb484bf3b0098ee913e5b2b4
出典データセット
uspto-grants-2010_06
特許番号
US07745438B2

反応ノート

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