Acetonitrile → 4-(Biphenyl-2-yloxy)-3,5,6-trichlorophthalonitrile

HRID 525841

反応式

HRID 525841 の反応式
[Cl:1][C:2]1[C:3](Cl)=[C:4]([Cl:13])[C:5]([Cl:12])=[C:6]([C:10]#[N:11])[C:7]=1[C:8]#[N:9].[C:15]1([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]([OH:21])=[CH:17][CH:18]=[CH:19][CH:20]=1.C(=O)([O-])[O-].[K+].[K+].C(#N)C>C(OCC)(=O)C>[C:15]1([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[O:21][C:3]1[C:2]([Cl:1])=[C:7]([C:8]#[N:9])[C:6](=[C:5]([Cl:12])[C:4]=1[Cl:13])[C:10]#[N:11]

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 7017(1,1'-Biphenyl)-2-olHCID 11430Potassium CarbonateHCID 160571,2-Benzenedicarbonitrile, 3,4,5,6-tetrachloro-

生成物 1

HCID 1179027074-(Biphenyl-2-yloxy)-3,5,6-trichlorophthalonitrile

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a 250 mL flask, 4.8 g of tetrachlorophthalonitrile, 4.3 g of biphenyl-2-ol, 5 g of potassium carbonate (K2CO3) and 55 mL of acetonitrile are added, followed by heating for 12 hours while refluxing. After completion of the reaction, 30 mL of ethyl acetate is added and filtered to remove the solvent. To the obtained solid, a suitable amount of dichloromethane is added to dissolve the solid, followed by adding hexane for crystallization. The obtained solid is filtered and dried under vacuum to obtain a compound, 4-[(biphenyl-2-yl)oxy]-3,5,6-trichlorophthalonitrile. The second step reaction may be represented by Reaction Scheme 2:

後処理

  1. temperatureby heating for 12 hours
  2. temperaturewhile refluxing
  3. additionis added
  4. filtrationfiltered
  5. customto remove the solvent
  6. additionTo the obtained solid, a suitable amount of dichloromethane is added
  7. dissolutionto dissolve the solid
  8. additionby adding hexane
  9. customfor crystallization
  10. filtrationThe obtained solid is filtered
  11. customdried under vacuum

出典と根拠

ORDレコード
ord-9f221331d5624b8793ac8825c68b4545
出典データセット
uspto-grants-2016_05
特許番号
US09341743B2

関連ノート

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