Potassium Carbonate → HCID 19963111, compound

HRID 52144Notes

Reaction equation

HRID 52144 reaction equation
[CH3:1][C:2]1[C:3]([CH2:20][S:21][C:22]2[NH:26][C:25]3[CH:27]=[CH:28][CH:29]=[CH:30][C:24]=3[N:23]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][N:14](C(=O)C)[CH2:13][CH2:12]1.C(=O)([O-])[O-].[K+].[K+]>Cl>[CH3:1][C:2]1[C:3]([CH2:20][S:21][C:22]2[NH:23][C:24]3[CH:30]=[CH:29][CH:28]=[CH:27][C:25]=3[N:26]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1

Participants

4

Conditions

Temperature
50 °C

Procedure

2-((3-Methyl-4-(2-(4-acetylpiperazin1-yl)ethylthio)-2-pyridyl)methylthio)-1H-benzimidazole (38 g) was dissolved in 6N hydrochloric acid and the mixture was stirred at 50° C. for 2 hours. After the completion of the reaction, the mixture was made alkaline with potassium carbonate and extracted with a mixed solvent of chloroform-methanol. The chloroform-methanol layer was dried over anhydrous magnesium sulfate, the solvent was distilled away and the residue was recrystallized from ethanol to give 2-((3-methyl-4-(2-(piperazin1-yl)ethylthio)-2-pyridyl)methylthio)-1H-benzimidazole as crystals, melting point 166°-168° C.

Workup

  1. customAfter the completion of the reaction
  2. extractionextracted with a mixed solvent of chloroform-methanol
  3. dry with materialThe chloroform-methanol layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled away
  5. customthe residue was recrystallized from ethanol

Sources & evidence

ORD record
ord-38e916ca168249729a81f5c06ab89353
Source dataset
uspto-grants-1997_04
Patent number
US05616581

Reaction notes

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