Reaktionsgleichung
[NH2:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH:4]=O.[NH2:11][C:12](N)=[O:13]>>[Cl:10][C:8]1[CH:9]=[C:2]2[C:3]([CH:4]=[N:11][C:12]([OH:13])=[N:1]2)=[CH:6][CH:7]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 170 °C
Versuchsvorschrift
In a 500 mL round bottom flask, the uniform mixture of 2-amino-4-chlorobenzaldehyde (16 g, 103.2 2 mmol) and urea (123.8 g, 2063 mmol) was heated at 170° C. with vigorous stirring for 2 h. On completion of reaction, the reaction mixture was cooled to rt and diluted with ice-cold water. The solid that formed was collected by filtration and washed with ice-cold water. The solid was dried under reduced pressure to give crude 7-chloroquinazolin-2-ol as a yellow solid. Yield: 19 g. LCMS (ESI, m/z): 181 (M+1)+
Aufarbeitung
- customOn completion of reaction
- temperaturethe reaction mixture was cooled to rt
- additiondiluted with ice-cold water
- customThe solid that formed
- filtrationwas collected by filtration
- washwashed with ice-cold water
- customThe solid was dried under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-b28a4f0b61c14aa5a3ef1d4a8e03b04b
- Quelldatensatz
- uspto-grants-2016_04
- Patentnummer
- US09303028B2
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