Hydrochloric Acid → HCID 136029126, compound

HRID 728802Notes

Reaction equation

HRID 728802 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+]>>[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

4

Reactant 3

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

Product 1

HCID 136029126HCID 136029126, compound

Procedure

A mixture of 2-amino-9-[(2,5-dimethyl-3-thienyl)methyl]-6-chloropurine (3.8g, 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. filtrationfiltered
  6. customto give 3.6 g
  7. customAn analytical sample was obtained by chromatography over silica gel using 10% methanol/chloroform
  8. washas eluting solvent, mp>300° C. (dec)

Sources & evidence

ORD record
ord-0f2a6d1d70354b8cb2617474a7467f71
Source dataset
uspto-grants-1991_09
Patent number
US05051429

Reaction notes

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