Reaktionsgleichung
CO[C:3](=[O:18])[CH:4]([O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[O:16][CH3:17])[C:5]([O:7]C)=O.C[O-].[Na+].Cl.[C:23]([NH2:26])(=[NH:25])[CH3:24]>CO>[CH3:17][O:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[O:9][C:4]1[C:3]([OH:18])=[N:25][C:23]([CH3:24])=[N:26][C:5]=1[OH:7]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A solution of 10 g of dimethyl-(o-methoxyphenoxy)malonate (Example 1b) in 80 ml dry methanol was cooled to 0° C. 6.71 g of sodium methylate was added portionenwise. To the suspension was added 2.84 g of acetamidine hydrochloride and the mixture was stirred overnight at room temperature. The solvent was removed under reduced pressure and the residue was suspended in 100 ml of diethyl ether. The solid was filtered off, washed with another portion of 100 ml of diethyl ether and dissolved in 50 ml of water. The pH was adjusted to 4 by adding 25 ml of glacial acetic acid. The white precipitate that formed was filtered off, washed with water and dried to yield 5.17 g of 5-(o-methoxyphenoxy)-4,6-dihydroxy-2-methyl-pyrimidine (or a tautomer) as a white powder.
Aufarbeitung
- customThe solvent was removed under reduced pressure
- filtrationThe solid was filtered off
- washwashed with another portion of 100 ml of diethyl ether
- dissolutiondissolved in 50 ml of water
- additionby adding 25 ml of glacial acetic acid
- customThe white precipitate that formed
- filtrationwas filtered off
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-eab1ffd049c04bde8e2f3cc6f0bead7e
- Quelldatensatz
- uspto-grants-2004_04
- Patentnummer
- US06720322B2
Verknüpfte Notizen
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