N,N-二甲基甲酰胺 → 5-[N-(4-formylphenyl)-N-(4-tolyl)amino]acenaphthene

HRID 1954

反应方程式

HRID 1954 反应方程式
[C:1]1([CH3:26])[CH:6]=[CH:5][C:4]([N:7]([C:14]2[C:24]3[C:25]4[C:17]([CH2:18][CH2:19][C:20]=4[CH:21]=[CH:22][CH:23]=3)=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:3][CH:2]=1.P(Cl)(Cl)(Cl)=O.[OH-:32].[Na+].[CH3:34]N(C)C=O>O>[CH:26]([C:1]1[CH:6]=[CH:5][C:4]([N:7]([C:14]2[C:24]3[C:25]4[C:17]([CH2:18][CH2:19][C:20]=4[CH:21]=[CH:22][CH:23]=3)=[CH:16][CH:15]=2)[C:8]2[CH:9]=[CH:10][C:11]([CH3:34])=[CH:12][CH:13]=2)=[CH:3][CH:2]=1)=[O:32]

参与物

6

反应物 4

HCID 6228N,N-二甲基甲酰胺HCID 14798二甲基对苯二胺二盐酸HCID 24813三氯氧磷HCID 196889135-[N-(4-tolyl)-N-phenylamino]acenaphthene2 次

产物 1

HCID 196889185-[N-(4-formylphenyl)-N-(4-tolyl)amino]acenaphthene收率 97.1%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
50 °C

实验过程

4.7 g (0.014 mol) of the above prepared 5-[N-(4-tolyl)-N-phenylamino]acenaphthene was dissolved in 30 ml of N,N-dimethylformamide, and 3.22 g (0.021 mol) of phosphorus oxychloride was dropwise added thereto at room temperature for 10 minutes. After the temperature was raised to 50° C., and the mixture was stirred for 14 hours. The reaction was determined to be finished when disappearance of 5-[N-(4-tolyl)-N-phenylamino]acenaphthene was identified. The reaction product was poured into an aqueous solution having 10 g (0.23 mol) of 93% sodium hydroxide dissolved in 250 ml of water. The resultant mixture was cooled to precipitate a crystal, which was then filtrated, washed with water and dried to obtain 4.94 g (yield: 97.1%) of 5-[N-(4-formylphenyl)-N-(4-tolyl)amino]acenaphthene.

后处理

  1. additionThe reaction product was poured into an aqueous solution
  2. customto precipitate a crystal, which
  3. filtrationwas then filtrated
  4. washwashed with water
  5. customdried

来源与证据

ORD记录
ord-20078ac392344345839361b7b292e056
来源数据集
uspto-grants-1998_03
专利号
US05728500

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