Phosphorus oxychloride → HCID 89654102, Verbindung
Reaktionsgleichung
[ClH:1].[CH3:2][C:3]1([CH3:9])[NH:7][NH:6][C:5](=O)[CH2:4]1.O=P(Cl)(Cl)[Cl:12]>>[ClH:12].[Cl:1][C:5]1[CH2:4][C:3]([CH3:9])([CH3:2])[NH:7][N:6]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 90 °C
Versuchsvorschrift
A round 50 mL round bottom flask equipped with stir bar, Vigreux column and nitrogen inlet was charged with 5,5-dimethyl-pyrazolidin-3-one.Hydrochloride (300 mg, 2.0 mmol) and POCl3 (4 mL). The mixture was heated at 90° C. for 3 h. LC-MS showed consumption of SM. The POCl3 was evaporated under reduced pressure and trace POCl3 was removed under high vacuum for 30 min. Amount obtained: 336 mg, 2.0 mmol, 100% yield. The material was used as in the next step. Step 4
Aufarbeitung
- customA round 50 mL round bottom flask equipped
- customconsumption of SM
- customThe POCl3 was evaporated under reduced pressure and trace POCl3
- customwas removed under high vacuum for 30 min
- customAmount obtained
Quellen und Nachweise
- ORD-Eintrag
- ord-dc887be935324e6fa66dc1fca179e980
- Quelldatensatz
- uspto-grants-2014_07
- Patentnummer
- US08791114B2
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