Perchloric Acid → HCID 13151607, compound

HRID 2290248Notes

Reaction equation

HRID 2290248 reaction equation
Cl(O)(=O)(=O)=O.[CH2:6]([N:10]1[C:19](=[O:20])[C:18]2[N:17]([CH2:21][CH2:22][CH:23]3[O:25][CH2:24]3)[CH:16]=[N:15][C:14]=2[N:13]([CH2:26][CH2:27][CH2:28][CH3:29])[C:11]1=[O:12])[CH2:7][CH2:8][CH3:9].C(=O)(O)[O-:31].[Na+]>COCCOC.O>[CH2:6]([N:10]1[C:19](=[O:20])[C:18]2[N:17]([CH2:21][CH2:22][CH:23]([OH:31])[CH2:24][OH:25])[CH:16]=[N:15][C:14]=2[N:13]([CH2:26][CH2:27][CH2:28][CH3:29])[C:11]1=[O:12])[CH2:7][CH2:8][CH3:9]

Participants

5

Reactant 3

HCID 24247Perchloric AcidHCID 516892Sodium BicarbonateHCID 13151640HCID 13151640, compound

Product 1

HCID 13151607HCID 13151607, compound

Reagents, catalysts & solvents 1

HCID 18180031Water 1,2-dimethoxyethaneSolvent

Procedure

0.4 ml of perchloric acid (70% strength) was added dropwise with stirring in 5 minutes to a solution of 7 g of 1,3-dibutyl-7-(3,4-epoxybutyl)xanthine in 300 ml of a mixture of ethylene glycol dimethyl ether/water (volume ratio 3:2) at room temperature. After stirring at room temperature for 45 hours, the mixture was neutralized with sodium bicarbonate and the solution was evaporated. The residue was taken up with methylene chloride and purified by column chromatography on silica gel with a mixture of chloroform and ethanol (volume ratio 8:2) as the mobile phase and by recrystallization from methylene chloride/petroleum ether.

Workup

  1. customthe solution was evaporated
  2. custompurified by column chromatography on silica gel with a mixture of chloroform and ethanol (volume ratio 8:2) as the mobile phase and by recrystallization from methylene chloride/petroleum ether

Sources & evidence

ORD record
ord-8aa8512118cc43deb56ee96efab4e737
Source dataset
uspto-grants-1986_10
Patent number
US04616020

Reaction notes

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