Acetonitrile → Methyl 4-(2,3,6-trichloro-4,5-dicyano-phenoxy)benzoate

HRID 525840

反応式

HRID 525840 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].[OH:15][C:16]1[CH:25]=[CH:24][C:19]([C:20]([O:22][CH3:23])=[O:21])=[CH:18][CH:17]=1.C(=O)([O-])[O-].[K+].[K+].C(#N)C>C(OCC)(=O)C>[Cl:13][C:4]1[C:5]([Cl:12])=[C:6]([C:10]#[N:11])[C:7]([C:8]#[N:9])=[C:2]([Cl:1])[C:3]=1[O:15][C:16]1[CH:17]=[CH:18][C:19]([C:20]([O:22][CH3:23])=[O:21])=[CH:24][CH:25]=1

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 7456MethylparabenHCID 11430Potassium CarbonateHCID 160571,2-Benzenedicarbonitrile, 3,4,5,6-tetrachloro-

生成物 1

HCID 117902339Methyl 4-(2,3,6-trichloro-4,5-dicyano-phenoxy)benzoate

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, 3.98 g of methyl 4-hydroxybenzoate, 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, methyl 4-(2,3,6-trichloro-4,5-dicyano-phenoxy)benzoate. The first step reaction may be represented by Reaction Scheme 1:

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-91f652bde2d144b8bcc88d059b1c6ca6
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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