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Hydrochloric Acid → 3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole hydrochloride

HRID 542870
Notes
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Reaction equation

HRID 542870 reaction equation
[ClH:1].[CH2:2]([C:4]1[N:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:7]([C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=2)=[N:6][N:5]=1)[CH3:3].C(OC(C)C)(C)C>C(O)C>[ClH:1].[CH2:2]([C:4]1[N:8]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:7]([C:15]2[CH:16]=[CH:17][C:18]([O:21][CH3:22])=[CH:19][CH:20]=2)=[N:6][N:5]=1)[CH3:3]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 7914Diisopropyl EtherHCID 130540223-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole

Product 1

HCID 201515513-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole hydrochloride

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

2.85 ml of a 6.4N hydrogen chloride solution in ethanol were added to a solution of 5.1 g of the product of Example 6 in 5.1 ml of ethanol and then isopropyl ether was added thereto. The mixture was filtered and the recovered product was empasted several times with isopropyl ether, filtered and was dried. The product was dissolved in 350 ml of tetrahydrofuran and the solution was filtered and concentrated to a volume of 75 ml. The mixture was cooled, iced and filtered and the recovered product was washed with tetrahydrofuran and dried to obtain 3.3 g of 3-ethyl-5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole hydrochloride melting towards 150° C. with decomposition.

Workup

  1. filtrationThe mixture was filtered
  2. filtrationfiltered
  3. customwas dried
  4. dissolutionThe product was dissolved in 350 ml of tetrahydrofuran
  5. filtrationthe solution was filtered
  6. concentrationconcentrated to a volume of 75 ml
  7. temperatureThe mixture was cooled
  8. filtrationiced and filtered
  9. washthe recovered product was washed with tetrahydrofuran
  10. customdried

Sources & evidence

ORD record
ord-62c3bd1087044bac95b710b6c602a40b
Source dataset
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04659729

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes