Ethyl Acetate → HCID 14748460, compound

HRID 1904906Notes

Reaction equation

HRID 1904906 reaction equation
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH2:11][CH2:12][C:13](=[N:15][OH:16])[NH2:14])[C:6]=2[C:5](=[O:17])[NH:4][C:3]1=[O:18].[C:19](OCC)(=O)[CH3:20].[Na]>C(O)C>[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH2:11][CH2:12][C:13]3[N:14]=[C:19]([CH3:20])[O:16][N:15]=3)[C:6]=2[C:5](=[O:17])[NH:4][C:3]1=[O:18]

Participants

5

Reactant 3

HCID 8857Ethyl AcetateHCID 5360545SodiumHCID 86743155HCID 86743155, compound

Product 1

HCID 14748460HCID 14748460, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 2.52 g of 3-(3-methyl-xanthine-7-yl)propionic acid amide oxime, 4.0 ml of ethyl acetate and a solution of 0.46 g of metallic sodium in 25 ml of ethanol is heated to boiling under stirring for 5 hours. The hot reaction mixture is filtered and the filtrate is evaporated. The residue is treated with 20 ml of water, the pH is adjusted to 7 and the precipitated product is crystallized from water. Thus 1.7 g of 3.7-dihydro-3-methyl-7-(2-[5-methyl-1,2,4-oxadiazole-3-yl]-ethane-1-yl)-1H-purine-2,6-dione are obtained, m.p.: 258°-260° C.

Workup

  1. filtrationThe hot reaction mixture is filtered
  2. customthe filtrate is evaporated
  3. additionThe residue is treated with 20 ml of water
  4. customthe precipitated product is crystallized from water

Sources & evidence

ORD record
ord-41f0e5d2859e4ce4b6dc38b34f42e403
Source dataset
uspto-grants-1989_06
Patent number
US04840949

Reaction notes

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