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

HRID 525840
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HRID 525840 반응식
[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
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참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate
용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-91f652bde2d144b8bcc88d059b1c6ca6
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09341743B2

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