Hydrochloric Acid → HCID 67182077, compound

HRID 2403887Notes

Reaction equation

HRID 2403887 reaction equation
[CH2:1]([O:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:23]C)[N:12]2[CH2:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][NH:18]2)=[C:8]([NH2:25])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl>O1CCOCC1>[NH2:25][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:23])[N:12]2[CH2:15][CH2:16][CH:17]1[CH2:22][CH2:21][CH2:20][CH2:19][NH:18]1

Participants

4

Reactant 2

HCID 313Hydrochloric Acid2×HCID 67183075HCID 67183075, compound

Product 1

HCID 67182077HCID 67182077, compoundYield 54%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

The crude aqueous solution containing approx 45 mg 2-(butyloxy)-8-(methyloxy)-9-[2-(2-piperidinyl)ethyl]-9H-purin-6-amine (45 mg, 0.129 mmol) was treated with a solution of HCl in 1,4-dioxane (0.807 mL, 3.23 mmol, 4 molar solution). This was stirred at ambient temperature in a capped vial overnight to give a pale solution. A further 1 ml of 4 molar HCl solution in 1,4-dioxane was added and stirring continued over the weekend. The yellow reaction solution was evaporated to dryness under N2 in a blow down unit. The residue was purified by MDAP (Method A), appropriate fractions were evaporated under N2 in a blow down unit to give the title compound as a white solid (23.3 mg).

Workup

  1. customto give a pale solution
  2. stirringstirring
  3. customThe yellow reaction solution was evaporated to dryness under N2 in a blow down unit
  4. customThe residue was purified by MDAP (Method A), appropriate fractions
  5. customwere evaporated under N2 in a blow down unit

Sources & evidence

ORD record
ord-aebab575af24446c904b8f843023917f
Source dataset
uspto-grants-2014_08
Patent number
US08802684B2

Reaction notes

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