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Nitromethane → HCID 55250532、化合物

HRID 1963074
ノート
印刷プレビュー

反応式

HRID 1963074 の反応式
[F:1][C:2]1[C:3]([CH3:10])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=O.[N+:11]([CH3:14])([O-:13])=[O:12].C([O-])(=O)C.[NH4+]>C(O)(=O)C>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:4](/[CH:5]=[CH:14]/[N+:11]([O-:13])=[O:12])[C:3]=1[CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6375NitromethaneHCID 517165Ammonium AcetateHCID 27792353-Fluoro-2-methylbenzaldehyde

生成物 1

HCID 55250532HCID 55250532、化合物収率 89%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A Knoevenagel condensation was carried out by stirring 3-fluoro-2-methyl-benzaldehyde (20.721 g, 150 mmol), nitromethane (48.75 ml, 900 mmol) and ammonium acetate (34.687 g, 450 mmol) in 300 ml of acetic acid at 115° C. for 3.5 h. The mixture was evaporated to dryness under reduced pressure and the residue was dissolved in 250 ml of EA. The solution was washed with water (250 ml), three times with a 1 N sodium hydroxide solution (125 ml) and with brine (125 ml), dried over magnesium sulfate, filtered and evaporated to dryness. 24.18 g of the title compound were obtained as a yellow solid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customA Knoevenagel condensation
  2. customThe mixture was evaporated to dryness under reduced pressure
  3. dissolutionthe residue was dissolved in 250 ml of EA
  4. washThe solution was washed with water (250 ml), three times with a 1 N sodium hydroxide solution (125 ml) and with brine (125 ml)
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-f5896acb88f6439195860fde8793f111
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08415336B2

反応ノート

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