Hydrochloric Acid → HCID 136029126, compound

HRID 1710191Notes

Reaction equation

HRID 1710191 reaction equation
[NH2:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][C:12]2[CH:16]=[C:15]([CH3:17])[S:14][C:13]=2[CH3:18])=[C:4](Cl)[N:3]=1.Cl.[OH-:21].[Na+]>C(O)(=O)C>[CH3:18][C:13]1[S:14][C:15]([CH3:17])=[CH:16][C:12]=1[CH2:11][N:8]1[CH:7]=[N:6][C:5]2[C:4](=[O:21])[NH:3][C:2]([NH2:1])=[N:10][C:9]1=2

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 14306334HCID 14306334, compound

Product 1

HCID 136029126HCID 136029126, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture of 2-amino-9-[(2,5-dimethyl-3-thienyl)methyl]-6-chloropurine (3.8 g, 0.0129 mol) and 2N HCl was heated on a steambath for 3.0 hours and then heated under reflux for another hour. At the end of this time 1N NaOH solution was added to the solution till basic and the mixture was heated for another five minutes. The mixture was then acidified with acetic acid, cooled, and filtered to give 3.6 g, of the product. An analytical sample was obtained by chromatography over silica gel using 10% methanol/chloroform as eluting solvent, mp >300° C. (dec).

Workup

  1. temperaturewas heated on a steambath for 3.0 hours
  2. temperatureheated
  3. temperatureunder reflux for another hour
  4. temperaturewas heated for another five minutes
  5. temperaturecooled
  6. filtrationfiltered
  7. customto give 3.6 g
  8. customAn analytical sample was obtained by chromatography over silica gel using 10% methanol/chloroform
  9. washas eluting solvent, mp >300° C. (dec)

Sources & evidence

ORD record
ord-6c474eea0b1e4255a99db638e2a8926e
Source dataset
uspto-grants-1990_08
Patent number
US04952693

Reaction notes

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