Hydrochloric Acid → HCID 57699842, compound

HRID 1011203Notes

Reaction equation

HRID 1011203 reaction equation
[CH2:1]([NH:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:25]C)[N:12]2[CH2:15][CH2:16][CH:17]2[CH2:22][CH2:21][O:20][C:19]([CH3:24])([CH3:23])[CH2:18]2)=[C:8]([NH2:27])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl.O1CCOCC1>CO>[NH2:27][C:8]1[N:7]=[C:6]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:14]=[C:13]2[C:9]=1[NH:10][C:11](=[O:25])[N:12]2[CH2:15][CH2:16][CH:17]1[CH2:22][CH2:21][O:20][C:19]([CH3:24])([CH3:23])[CH2:18]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 57699793HCID 57699793, compound

Product 1

HCID 57699842HCID 57699842, compoundYield 99.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of N2-butyl-9-[2-(2,2-dimethyltetrahydro-2H-pyran-4-yl)ethyl]-8-(methyloxy)-9H-purine-2,6-diamine (135 mg, 0.359 mmol) in methanol (10 ml) was added 4M HCl solution in dioxane (2.241 ml, 8.96 mmol) and the mixture was left standing at 20° C. After 6 hours the solvent was evaporated under a stream of nitrogen. The residue was loaded in methanol onto a 10 g aminopropyl SPE cartridge and eluted with methanol. The solvent was removed by evaporation to give the title compound (129 mg).

Workup

  1. waitthe mixture was left
  2. customstanding at 20° C
  3. customAfter 6 hours the solvent was evaporated under a stream of nitrogen
  4. washeluted with methanol
  5. customThe solvent was removed by evaporation

Sources & evidence

ORD record
ord-ea533ec09cee4e4199058062c068b02f
Source dataset
uspto-grants-2011_07
Patent number
US07977344B2

Reaction notes

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