Diethyl Ether → HCID 70601464, compound
Reaction equation
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([O:18][CH3:19])=[C:6]([C:8]2[N:16]=[C:15]3[C:11](=[N:12][N:13]=[N:14]3)[C:10](=[O:17])[N:9]=2)[CH:7]=1.C(OCC)C.[C:25]([CH2:28][C:29](=O)[CH3:30])(=[O:27])[CH3:26]>>[C:25]([CH:28]=[C:29]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([O:18][CH3:19])=[C:6]([C:8]2[N:16]=[C:15]3[C:11](=[N:12][N:13]=[N:14]3)[C:10](=[O:17])[N:9]=2)[CH:7]=1)[CH3:30])(=[O:27])[CH3:26]Participants
4
Procedure
A stirred suspension of 2-(5-amino-2-methoxyphenyl)-8-azapurin-6-one (1.34 g) in acetylacetone (15 ml) was heated at reflux for one hour. The mixture was then cooled and poured into diethyl ether (100 ml). The precipitated solid was filtered off and recrystallised twice from ethanol with the aid of charcoal to give 2-[5-(1-acetylprop-1-en-2-ylamino)-2-methoxyphenyl]-8-azapurin-6-one (1.2 g), m.p. 239°-240° C. (with decomposition).
Workup
- temperaturewas heated
- temperatureat reflux for one hour
- temperatureThe mixture was then cooled
- filtrationThe precipitated solid was filtered off
- customrecrystallised twice from ethanol with the aid of charcoal
Sources & evidence
- ORD record
- ord-74014326d6e94ba4b9b282d00fb758bb
- Source dataset
- uspto-grants-1979_09
- Patent number
- US04167568
Reaction notes
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