Ethanol → HCID 18706827, Verbindung

Temperatur

70 °C

To 2-amino-6-chloro-5-[(p-chlorophenyl)azo]-4-[(2-hydroxyethyl)amino]pyrimidine (3.0 g, 9.2 mmol) were added ethanol (76.0 ml), water (76.0 ml) and acetic acid (8.0 ml), and the mixture was heated to 70° C. A zinc powder (7.52 g) was added portionwise with stirring in a nitrogen stream and the mixture was stirred at the same temperature for 1.5 hours to give a solution. The reaction mixture was filtered and the solvent of the filtrate was distilled away under reduced pressure. Water was added to the residue and the mixture was extracted with chloroform, washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography (chloroform:methanol=20:1) to give pale-brown crystals (0.34 g, 18.3%), m.p. 164-167° C.

1. stirringthe mixture was stirred at the same temperature for 1.5 hours
2. customto give a solution
3. filtrationThe reaction mixture was filtered
4. distillationthe solvent of the filtrate was distilled away under reduced pressure
5. additionWater was added to the residue
6. extractionthe mixture was extracted with chloroform
7. washwashed with water
8. dry with materialdried over anhydrous magnesium sulfate
9. distillationThe solvent was distilled away under reduced pressure
10. customthe residue was purified by silica gel column chromatography (chloroform:methanol=20:1)

ORD-Eintrag

ord-e8ef4d89e24c417c9dff18b611897c93

Quelldatensatz

uspto-grants-2000_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06080750