Acetic Acid → 2-({[(4-Fluorophenyl)(phenyl)methyl]amino}methylidene)butanedinitrile

HRID 730423ノート

反応式

HRID 730423 の反応式
[K].[CH:2]([CH:4]([CH2:7][C:8]#[N:9])[C:5]#[N:6])=O.[F:10][C:11]1[CH:16]=[CH:15][C:14]([CH:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[NH2:18])=[CH:13][CH:12]=1.C(O)(=O)C>O>[F:10][C:11]1[CH:12]=[CH:13][C:14]([CH:17]([NH:18][CH:2]=[C:4]([CH2:7][C:8]#[N:9])[C:5]#[N:6])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:15][CH:16]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 111832724-Fluoro-α-phenylbenzenemethanamineHCID 86606793HCID 86606793、化合物

生成物 1

HCID 690558642-({[(4-Fluorophenyl)(phenyl)methyl]amino}methylidene)butanedinitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

To a solution of formyl succinonitrile potassium salt (7.26 g, 49.7 mmol) and 1-(4-fluorophenyl)-1-phenylmethaneamine (11.0 g, 54.7 mmol) in water-(20 ml) was added acetic acid (20 ml) at room temperature, the mixture was stirred at 100° C. for 30 minutes, and the solvent was distilled off under reduced pressure. The residue was poured into iced water, made basic by adding potassium carbonate and then extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give the objective product as a solid material.

後処理

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionThe residue was poured into iced water
  3. additionby adding potassium carbonate
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-3fbc576e9c1547baab609e75c9ee59f5
出典データセット
uspto-grants-2009_09
特許番号
US07582651B2

反応ノート

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