Formaldehyde → HCID 13115425、化合物

HRID 1075320ノート

反応式

HRID 1075320 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:11][C:12]([NH:14][C:15](C)=O)=[O:13].C=O>S(=O)(=O)(O)O>[CH3:10][C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]=1[CH2:15][NH:14][C:12](=[O:13])[CH3:11]

参加物

5

反応物 3

HCID 712FormaldehydeHCID 74734-NitrotolueneHCID 12263Diacetamide

生成物 1

HCID 13115425HCID 13115425、化合物収率 65%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
55 °C

実験手順

To a solution of p-nitrotoluene (2.74 g; 0.02 mol) and diacetamide (4.24 g; 0.04 mol) in concentrated sulfuric acid (20 ml) is added aqueous formaldehyde (37%; 1.6 g; 0.02 mol) dropwise with stirring. The reaction mixture is stirred at room temperature for 17 hours, heated to 55° C. for 8 hours and then to 85° C. for 19 hours. The mixture is then poured onto ice. The resulting colorless precipitate is removed by filtration and recrystallized from aqueous ethanol to give 2.7 g of product (65% yield) having a melting point of 133° to 137.5° C.

後処理

  1. stirringThe reaction mixture is stirred at room temperature for 17 hours
  2. additionThe mixture is then poured onto ice
  3. customThe resulting colorless precipitate is removed by filtration
  4. customrecrystallized from aqueous ethanol

出典と根拠

ORDレコード
ord-e87131df6bfa48e1bf1bef72c29fee39
出典データセット
uspto-grants-1983_07
特許番号
US04395577

反応ノート

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