Potassium Hydroxide → HCID 18436985, compound

HRID 456535Notes

Reaction equation

HRID 456535 reaction equation
[OH-].[K+].[CH2:3]([N:10]1[CH2:15][CH2:14][N:13]([C:16]2[C:17]3[S:33][CH:32]=[CH:31][C:18]=3[N:19](S(C3C=CC(C)=CC=3)(=O)=O)[N:20]=2)[CH2:12][CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>CO>[CH2:3]([N:10]1[CH2:15][CH2:14][N:13]([C:16]2[C:17]3[S:33][CH:32]=[CH:31][C:18]=3[NH:19][N:20]=2)[CH2:12][CH2:11]1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

Participants

4

Procedure

To a stirred mixture of KOH(s) (56.09 g, 2.66 mol) in methyl 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-7559bfbe73df49ed914ccbd360f2f340
Source dataset
uspto-grants-2007_03
Patent number
US07186724B2

Reaction notes

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