Potassium Hydroxide → HCID 18436985, compound

HRID 2111722Notes

Reaction equation

HRID 2111722 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 taken 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-c74eec29c97749ac8cebb2072a4e2dfb
Source dataset
uspto-grants-2009_04
Patent number
US07521445B2

Reaction notes

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