Potassium Carbonate → HCID 22446289, compound

HRID 2024Notes

Reaction equation

HRID 2024 reaction equation
[CH3:1][O:2][CH2:3][CH2:4][N:5]1[C:13]2[C:12](=[O:14])[NH:11][C:10](=[O:15])[N:9]([CH3:16])[C:8]=2[N:7]=[CH:6]1.Cl[CH2:18][CH2:19][CH2:20][CH2:21][P:22]([O:27][CH2:28][CH3:29])(=[O:26])[O:23][CH2:24][CH3:25].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:1][O:2][CH2:3][CH2:4][N:5]1[C:13]2[C:12](=[O:14])[N:11]([CH2:18][CH2:19][CH2:20][CH2:21][P:22](=[O:26])([O:27][CH2:28][CH3:29])[O:23][CH2:24][CH3:25])[C:10](=[O:15])[N:9]([CH3:16])[C:8]=2[N:7]=[CH:6]1

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 19689195Diethyl(4-chlorobutyl)phosphonateHCID 543921147-Methoxyethyl-3-methylxanthine

Product 1

HCID 22446289HCID 22446289, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Conditions

Temperature
70 °C

Procedure

9 g (0.04 mol) of 7-methoxyethyl-3-methylxanthine were suspended in 100 ml of DMF, treated with 11 g (0.048 mol) of diethyl 4-chlorobutane-phosphonate and 10 g (0.064 mol) of activated potassium carbonate and heated at 70° C. for 4 hours. The solid was filtered off, the filtrate was concentrated under reduced pressure and the oily residue which remained was taken up in ethyl acetate, filtered again and crystallized from diisopropyl ether.

Workup

  1. filtrationThe solid was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. filtrationfiltered again
  4. customcrystallized from diisopropyl ether

Sources & evidence

ORD record
ord-1ccbe3ff71f04729a89ed7db3a53f3b8
Source dataset
uspto-grants-1998_03
Patent number
US05728686

Reaction notes

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