Acetic Acid → HCID 135670802, compound
Reaction equation
CS([C:5]1[N:10]=[C:9]2[N:11]=[C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH2:23][CH2:24][CH3:25])[NH:13][C:14](=[O:15])[C:8]2=[CH:7][N:6]=1)(=O)=O.[C:26](O)(=[O:28])[CH3:27]>[O-]CC.[Na+]>[CH2:26]([O:28][C:5]1[N:10]=[C:9]2[N:11]=[C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH2:23][CH2:24][CH3:25])[NH:13][C:14](=[O:15])[C:8]2=[CH:7][N:6]=1)[CH3:27]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A solution of 7-methylsulphonyl-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine (0.50 g) in sodium ethoxide solution (from sodium, 0.16 g, and ethanol, 25 ml) was stirred at ambient temperature for 1.5 hours. Cooling and acidification of the reaction mixture with glacial acetic acid (0.42 g) yielded a precipitate which was twice recrystallised from ethanol to yield the title compound, 0.29 g, m.p. 196°-197.5° C.
Workup
- temperatureCooling
- customwas twice recrystallised from ethanol
Sources & evidence
- ORD record
- ord-41143bea00864204967831f5ff974bd5
- Source dataset
- uspto-grants-1992_11
- Patent number
- US05162316
Reaction notes
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