Hydrochloric Acid → HCID 178422345, compound

HRID 248424Notes

Reaction equation

HRID 248424 reaction equation
C([N:4]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[N:6]2[N:13]=[C:14]([CH3:20])[C:15](SC(=O)C)=[C:5]12)(=O)C.Cl>C(O)C>[CH3:20][C:14]1[CH:15]=[C:5]2[NH:4][C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=3[N:6]2[N:13]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 19763717HCID 19763717, compound

Product 1

HCID 178422345HCID 178422345, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

4-Acetyl-3-acetylthio-2-methylpyrazolo[1,5-a]benzimidazole (2.0 g, 6.97 mmole) was added to a mixture of concentrated hydrochloric acid (5 ml) and ethanol (30 ml) and refluxed for 5 hr. A yellow solid precipitated during the heating period and was filtered off after cooling, 0.9 g. This was a mixture of several components, none of them being the required product, and was discarded. The ethanolic solution was poured into a solution of sodium bicarbonate (excess) in water (300 ml) and the white solid filtered off, washed and dried, 0.7 g, 61%, mp. 250°-252° C. IR and TLC (+ Dox spray test) comparison with authentic (6) showed the samples to be identical.

Workup

  1. temperaturerefluxed for 5 hr
  2. customA yellow solid precipitated during the heating period
  3. filtrationwas filtered off
  4. temperatureafter cooling
  5. additiona mixture of several components, none of them
  6. additionThe ethanolic solution was poured into a solution of sodium bicarbonate (excess) in water (300 ml)
  7. filtrationthe white solid filtered off
  8. washwashed
  9. customdried

Sources & evidence

ORD record
ord-010ecf86b0d745d299285e9a5ee9a41c
Source dataset
uspto-grants-1993_05
Patent number
US05210209

Reaction notes

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