Acetic Acid → HCID 178475805, compound

HRID 893941Notes

Reaction equation

HRID 893941 reaction equation
[OH:1][CH2:2][C:3]1[CH:15]=[C:14]2[N:5]([C:6](=[S:16])[NH:7][C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=32)[N:4]=1.[C:17](O)(=[O:19])[CH3:18]>C(OCC)(=O)C>[C:17]([O:1][CH2:2][C:3]1[CH:15]=[C:14]2[N:5]([C:6](=[S:16])[NH:7][C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=32)[N:4]=1)(=[O:19])[CH3:18]

Participants

4

Reactant 2

HCID 176Acetic AcidHCID 178519262HCID 178519262, compound

Product 1

HCID 178475805HCID 178475805, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

3.23 g (0.014 mole) of the product of Example 5 [2-(hydroxymethyl)pyrazolo[1,5-c]quinazoline-5(6H)-thione] is refluxed with 250 ml of glacial acetic acid for 20 hours under nitrogen. The solution is cooled and stripped to a solid residue which is dissolved in a mixture of ethyl acetate-absolute ethanol. The volume of solution is reduced and the concentrated solution set aside at 5°. The precipitate is filtered off to give the product. Recrystallization from ethyl acetate-absolute ethanol gives the title compound.

Workup

  1. temperatureThe solution is cooled
  2. customset aside at 5°
  3. filtrationThe precipitate is filtered off
  4. customto give the product
  5. customRecrystallization from ethyl acetate-absolute ethanol

Sources & evidence

ORD record
ord-9f424f86742046439412f7cdbbfae4c3
Source dataset
uspto-grants-1981_08
Patent number
US04282226

Reaction notes

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