Acetic Acid → HCID 12876546, compound
Reaction equation
[NH2:1][C:2]1[C:3](=[O:17])[N:4]([CH2:14][CH2:15][CH3:16])[C:5](=[O:13])[N:6]([CH2:9][CH:10]([OH:12])[CH3:11])[C:7]=1[NH2:8].[C:18](O)(=O)[CH3:19]>>[OH:12][CH:10]([CH3:11])[CH2:9][N:6]1[C:7]2[N:8]=[C:18]([CH3:19])[NH:1][C:2]=2[C:3](=[O:17])[N:4]([CH2:14][CH2:15][CH3:16])[C:5]1=[O:13]Participants
3
Procedure
About 15 g of 5,6-diamino-1-(2-hydroxypropyl)-3-propyl-2,4-(1H, 3H)-pyrimidinedione as an oil was refluxed for one hour in 50 ml of acetic acid. The solution was evaporated and the residue was dissolved in water. Active carbon was added and filtered off. To the filtrate 25 ml of 5-N NaOH was added and the solution was refluxed for 30 minutes. Hydrochloric acid was added until acid reaction and the received crystals were filtered off and recrystallized from 200 ml of water. Yield 2.7 g. NMR.
Workup
- customThe solution was evaporated
- dissolutionthe residue was dissolved in water
- additionActive carbon was added
- filtrationfiltered off
- additionTo the filtrate 25 ml of 5-N NaOH was added
- temperaturethe solution was refluxed for 30 minutes
- additionHydrochloric acid was added until acid reaction
- filtrationthe received crystals were filtered off
- customrecrystallized from 200 ml of water
Sources & evidence
- ORD record
- ord-303182d790b4458c95be689c0a3ee8b4
- Source dataset
- uspto-grants-1980_11
- Patent number
- US04233303
Reaction notes
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