HCID 20038772, compound → HCID 20038775, compound

HRID 1904265Notes

Reaction equation

HRID 1904265 reaction equation
[NH:1]1[CH:5]=[C:4]([NH:6][C:7]2[CH2:12][CH2:11][CH2:10][CH2:9][C:8]=2[C:13]([O:15]CC)=O)[CH:3]=[N:2]1>C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1>[O:15]=[C:13]1[C:8]2[CH2:9][CH2:10][CH2:11][CH2:12][C:7]=2[NH:6][C:4]2[CH:5]=[N:1][NH:2][C:3]1=2

Participants

3

Reactant 1

HCID 20038772HCID 20038772, compound

Product 1

HCID 20038775HCID 20038775, compoundYield 92%

Reagents, catalysts & solvents 1

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)Solvent

Procedure

Ethyl 2-(pyrazol-4-ylamino)cyclohexene-1-carboxylate (8.5 g, 0.036 mole) was added rapidly to refluxing Dowtherm A (250 ml) under nitrogen and the mixture heated under reflux for a further 15 minutes, before allowing to cool to room temperature. The mixture was diluted with 60°-80° petroleum ether (200 ml) and the solid then filtered off, washed well with petroleum ether and then ethanol, before drying under vacuum to give the title compound as a white solid (6.26 g, 92%), m.p. >325° C. Found: C, 63.20; H, 5.85; N, 22.20% C10H11N3O requires C, 63.50; H, 5.85; N, 22.20%

Workup

  1. temperaturethe mixture heated
  2. temperatureunder reflux for a further 15 minutes
  3. filtrationthe solid then filtered off
  4. washwashed well with petroleum ether
  5. dry with materialethanol, before drying under vacuum

Sources & evidence

ORD record
ord-7639087b4e8e4a55a2582d04910ed7e7
Source dataset
uspto-grants-1989_06
Patent number
US04837238

Reaction notes

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