Potassium Hydroxide → HCID 18436985, compound

HRID 1986929Notes

Reaction equation

HRID 1986929 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

Reactant 2

HCID 14797Potassium HydroxideHCID 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 is 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-a7f657025db3493f9130d6addb68e696
Source dataset
uspto-grants-2009_06
Patent number
US07550469B2

Reaction notes

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