Ethanol → HCID 21568428, Verbindung
Reaktionsgleichung
[CH3:1][CH2:2][O-:3].[Na+].Cl[C:6]1[N:7]=[C:8](Cl)[C:9]2[C:10](=[CH:12][S:13][CH:14]=2)[N:11]=1.[CH2:16]([OH:18])[CH3:17]>>[CH2:2]([O:3][C:6]1[N:7]=[C:8]([O:18][CH2:16][CH3:17])[C:9]2[C:10](=[CH:12][S:13][CH:14]=2)[N:11]=1)[CH3:1]Komponenten
4
Versuchsvorschrift
A solution of 0.06 mole sodium ethylate in ethyl alcohol is added dropwise while cooling to a suspension of 6.15 g (0.03 mole) of 2,4-dichloro-thieno[3,4-d]pyrimidine in 100 ml absolute ethyl alcohol. The speed of addition is regulated in such a way that the temperature of the reaction medium is maintained at between 0° and 5°C. When addition is completed, the solution is left to rise to room temperature and is then heated under reflux for 4 hours. It is then evaporated to dryness. The remaining solid is drained, washed with water and left to dry. AFter recrystallization from a 50/50 mixture of ethyl alcohol and water, 2.8 g (42% of theory) of 2,4-diethoxy-thieno[3,4-d]pyrimidine are obtained. M.P. 84°-86°C.
Aufarbeitung
- additionThe speed of addition
- temperatureis maintained at between 0° and 5°C
- additionWhen addition
- waitthe solution is left
- customto rise to room temperature
- temperatureis then heated
- temperatureunder reflux for 4 hours
- customIt is then evaporated to dryness
- washwashed with water
- waitleft
- customto dry
- customAFter recrystallization
- additionfrom a 50/50 mixture of ethyl alcohol and water, 2.8 g (42% of theory) of 2,4-diethoxy-thieno[3,4-d]pyrimidine
- customare obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-8d54416ca94146259b022d0adb7761cb
- Quelldatensatz
- uspto-grants-1976_01
- Patentnummer
- US03931204
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