Formaldehyde → HCID 13115425, 화합물

HRID 1075320노트

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HRID 1075320 반응식
[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]

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 74734-NitrotolueneHCID 12263Diacetamide

생성물 1

HCID 13115425HCID 13115425, 화합물수율 65%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
55 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e87131df6bfa48e1bf1bef72c29fee39
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04395577

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