Potassium Acetate → HCID 178458302, compound
Reaction equation
[NH2:1][C:2]1[N:3]=[C:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH2:17][CH2:18][CH3:19])[NH:5][C:6](=[O:9])[C:7]=1[NH2:8].C([O-])(=O)C.[K+].N[C:26](N)=[S:27]>>[CH2:17]([O:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[C:4]1[N:3]=[C:2]2[C:7](=[N:8][C:26]([SH:27])=[N:1]2)[C:6](=[O:9])[N:5]=1)[CH2:18][CH3:19]Participants
4
Conditions
- Temperature
- 175 °C
Procedure
A mixture of 4,5-diamino-2-(2-propoxyphenyl)pyrimidin-6-one (1.3 g), anhydrous potassium acetate (0.34 g) and thiourea (0.96 g) was heated at 170-180° C. for 2 hours. After digestion with water the mixture was filtered and the solid was dissolved in 1 Normal sodium hydroxide solution then re-precipitated by the addition of acetic acid. The dried solid was digested with chloroform and with ethanol to leave 1.12 g of a crude product. Repeated recrystallisations from dimethylformamide, 2-methoxyethanol, and acetic acid yielded the title compound, 0.32 g, m.p. 305-307° C.
Workup
- filtrationAfter digestion with water the mixture was filtered
- dissolutionthe solid was dissolved in 1 Normal sodium hydroxide solution
- customthen re-precipitated by the addition of acetic acid
- customto leave 1.12 g of a crude product
- customrecrystallisations from dimethylformamide, 2-methoxyethanol, and acetic acid
Sources & evidence
- ORD record
- ord-3c34b68a8a0444dca6ce8d571e411a89
- Source dataset
- uspto-grants-2001_03
- Patent number
- US06200980B1
Reaction notes
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