HCID 18436987, compound → HCID 18436985, compound

HRID 501309Notes

Reaction equation

HRID 501309 reaction equation
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:15]3[S:31][CH:30]=[CH:29][C:16]=3[N:17](S(C3C=CC(C)=CC=3)(=O)=O)[N:18]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CO>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:15]3[S:31][CH:30]=[CH:29][C:16]=3[NH:17][N:18]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

3

Reactant 1

HCID 18436987HCID 18436987, compound

Product 1

HCID 18436985HCID 18436985, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a stirred mixture of KOH(S) (56.09 g, 2.66 mol) in methly alcohol (1.33 L) is added 3-(4-benzyl-piperazin-1-yl)-1-(toluene-4-sulfonyl)-1H-thieno[3,2-c]pyrazole (241 g, 0.532 mol). The mixture is heated at reflux for 1.25 hours, cooled to room temperature and evaporated. The residue is taked up in EtOAc (1 L) washed with water (2 L), dried (MgSO4) filtered and evaporated. The residue was recrystallized from EtOAc/Heptane yielding 129 g (81%).

Workup

  1. temperatureThe mixture is heated
  2. temperatureat reflux for 1.25 hours
  3. customevaporated
  4. washwashed with water (2 L)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was recrystallized from EtOAc/Heptane yielding 129 g (81%)

Sources & evidence

ORD record
ord-a51da21ee0e442eda778a447af6bf972
Source dataset
uspto-grants-2010_08
Patent number
US07772252B2

Reaction notes

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