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HCID 15680277, compound → HCID 15680279, compound

HRID 2253883
Notes
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Reaction equation

HRID 2253883 reaction equation
[CH2:1]1[O:9][C:8]2[C:3](=[CH:4][CH:5]=[C:6]([C:22]([NH2:24])=O)[C:7]=2[C:10]2[C:11]([C:19]([NH2:21])=O)=[CH:12][CH:13]=[C:14]3[O:18][CH2:17][O:16][C:15]=23)[O:2]1>P(Cl)(Cl)(Cl)=O>[CH2:1]1[O:9][C:8]2[C:3](=[CH:4][CH:5]=[C:6]([C:22]#[N:24])[C:7]=2[C:10]2[C:11]([C:19]#[N:21])=[CH:12][CH:13]=[C:14]3[O:18][CH2:17][O:16][C:15]=23)[O:2]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 1

HCID 15680277HCID 15680277, compound

Product 1

HCID 15680279HCID 15680279, compoundYield 91.3%

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

5,6-Methylenedioxy-5',6'-methylenedioxy-2,2'-biphenyldicarboxamide (8 g) is refluxed in phosphorus oxychloride (70 ml) for 4 hours. The reaction mixture is cooled and then poured into ice water. The precipitated crystals are separated by filtration and dissolved in chloroform. The solution is washed with water, dried and distilled to remove the solvent to give 5,6-methylenedioxy-5',6'-methylenedioxy-2,2'-biphenyldicarbonitrile (6.5 g) as colorless crystal. M.p. 213°-215° C.

Workup

  1. temperature
The reaction mixture is cooled
  • customThe precipitated crystals are separated by filtration
  • dissolutiondissolved in chloroform
  • washThe solution is washed with water
  • customdried
  • distillationdistilled
  • customto remove the solvent
  • Sources & evidence

    ORD record
    ord-50560afea43143bb94b002adae0534d3
    Source dataset
    uspto-grants-1993_08
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US05233057

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes