Reaktionsgleichung
[Br:1][C:2]1[C:6]2[N:7]=[CH:8][NH:9][C:10](=O)[C:5]=2[S:4][CH:3]=1.O=P(Cl)(Cl)[Cl:14]>>[Br:1][C:2]1[C:6]2[N:7]=[CH:8][N:9]=[C:10]([Cl:14])[C:5]=2[S:4][CH:3]=1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 150 °C
Versuchsvorschrift
7-bromothieno[3,2-d]pyrimidin-4(3H)-one (5.9 g) was dissolved in POCl3 (20 mL) and the reaction mixture was stirred at 150° C. for 3 hours. The reaction mixture was cooled to room temperature, and remaining POCl3 was concentrated and placed in ice water. The solid thus obtained was washed with sodium bicarbonate and dried using nitrogen gas. The resulting compound was further dried over anhydrous sodium sulfate, and filtered and distilled under reduced pressure to obtain the title compound (1.0 g, 39%).
Aufarbeitung
- temperatureThe reaction mixture was cooled to room temperature
- concentrationwas concentrated
- customThe solid thus obtained
- washwas washed with sodium bicarbonate
- customdried
- dry with materialThe resulting compound was further dried over anhydrous sodium sulfate
- filtrationfiltered
- distillationdistilled under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-9247ec7529e84e45a198656acda7a568
- Quelldatensatz
- uspto-grants-2014_10
- Patentnummer
- US08853213B2
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