Phosphorus oxychloride → HCID 59447943, Verbindung
Reaktionsgleichung
[CH3:1][O:2][C:3]([C:5]1[CH:13]=[C:12]2[C:8]([C:9]3[C:17](O)=[N:16][CH:15]=[N:14][C:10]=3[NH:11]2)=[CH:7][CH:6]=1)=[O:4].O=P(Cl)(Cl)[Cl:21]>>[CH3:1][O:2][C:3]([C:5]1[CH:13]=[C:12]2[C:8]([C:9]3[C:17]([Cl:21])=[N:16][CH:15]=[N:14][C:10]=3[NH:11]2)=[CH:7][CH:6]=1)=[O:4]Komponenten
3
Reaktionsbedingungen
- Temperatur
- 90 °C
Versuchsvorschrift
A mixture of 4-hydroxy-9H-pyrimido[4,5-b]indole-7-carboxylic acid methyl ester (215 mg, 0.88 mmol) and POCl3 (2 mL) was heated at 90° C. for 2 hours. Upon cooling the reaction mixture was concentrated in vacuo to give the title compound and used immediately in the subsequent synthesis. LC-MS (1) Rt 1.79 min; m/z (ES+) 262/264.
Aufarbeitung
- temperatureUpon cooling the reaction mixture
- concentrationwas concentrated in vacuo