Acetic Anhydride → 3,8-Dimethyl-3,7-dihydro-1H-purine-2,6-dione
Reaction equation
[CH3:1][N:2]1[C:9]([NH2:10])=[C:8]([NH2:11])[C:6](=[O:7])[NH:5][C:3]1=[O:4].[C:12](OC(=O)C)(=O)[CH3:13]>>[CH3:1][N:2]1[C:9]2[N:10]=[C:12]([CH3:13])[NH:11][C:8]=2[C:6](=[O:7])[NH:5][C:3]1=[O:4]Participants
3
Procedure
A solution of 1-methyl-5,6-diaminouracil (2.5 g) in acetic anhydride (25 ml) was heated at reflux for 2 hours and then concentrated. The residue was dissolved in 10% sodium hydroxide solution (50 ml) and heated at reflux for 2 hours. After cooling to room temperature the solution was acidified to pH 4 with concentrated hydrochloric acid. The product was filtered, washed with water (15 ml), with acetone (15 ml) and then dried under vacuum. Yield 1.8 g.
Workup
- temperatureat reflux for 2 hours
- concentrationconcentrated
- dissolutionThe residue was dissolved in 10% sodium hydroxide solution (50 ml)
- temperatureheated
- temperatureat reflux for 2 hours
- filtrationThe product was filtered
- washwashed with water (15 ml), with acetone (15 ml)
- customdried under vacuum
Sources & evidence
- ORD record
- ord-844250ff3c3a466d861e7c252b8be194
- Source dataset
- uspto-grants-2000_06
- Patent number
- US06075029
Reaction notes
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