Hydrochloric Acid → HCID 25024973, compound

HRID 1011148Notes

Reaction equation

HRID 1011148 reaction equation
[CH2:1]([O:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:22]C)[N:12]2[CH2:15][CH:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[C:8]([NH2:24])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl.[OH-].[Na+]>CO.O1CCOCC1.O>[NH2:24][C:8]1[N:7]=[C:6]([O:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:14]=[C:13]2[C:9]=1[NH:10][C:11](=[O:22])[N:12]2[CH2:15][CH:16]1[CH2:17][CH2:18][O:19][CH2:20][CH2:21]1

Participants

7

Reactant 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 44248021HCID 44248021, compound

Product 1

HCID 25024973HCID 25024973, compoundYield 89.7%

Reagents, catalysts & solvents 3

HCID 887MethanolSolvent2×HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Procedure

2-Butoxy-8-methoxy-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purin-6-amine (0.22 g) was dissolved in methanol (10 mL) and treated with 4N hydrogen chloride in 1,4-dioxane (1 mL). The reaction was stirred at room temperature 16 hours and stripped to give a solid that was suspended in water (2 mL) before sufficient methanol was added until a solution was obtained. 2N Sodium hydroxide solution was added to bring to pH 7, and the solution concentrated until a suspension formed. The white solid was filtered and washed with water (2 mL, twice to complete transfer and wash). This was dried under suction and then under vacuum at 50° C. to give the title compound as a white solid (0.189 g).

Workup

  1. customto give a solid
  2. additionwas added until a solution
  3. customwas obtained
  4. concentrationthe solution concentrated until a suspension
  5. customformed
  6. filtrationThe white solid was filtered
  7. washwashed with water (2 mL
  8. washtwice to complete transfer and wash)
  9. customThis was dried under suction

Sources & evidence

ORD record
ord-3c18144918da40d9a70bddb1207b6ec8
Source dataset
uspto-grants-2011_07
Patent number
US07977344B2

Reaction notes

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