Reaktionsgleichung
[NH2:1][C:2]1[N:7]=[C:6](O)[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)[N:3]=1.P(Cl)(Cl)([Cl:17])=O.CN(C)C1C=CC=CC=1>>[Cl:17][C:6]1[CH:5]=[C:4]([C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)[N:3]=[C:2]([NH2:1])[N:7]=1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
32 g (170.04 mmol) of the compound (from example XXVIII) are dissolved in 87.1 ml (0.93 mmol) of phosphoryl chloride. 2.80 ml (22.11 mmol) of N,N-dimethylaniline are slowly added dropwise, and the mixture is stirred at 100° C. for one hour. The reaction solution is then stirred at room temperature for another two hours. The phosphoryl chloride is removed under reduced pressure using a rotary evaporator. Water/dichloromethane 9:1 is added to the residue, which is then boiled for 5 minutes. The mixture is then neutralized using saturated sodium bicarbonate solution and the product is filtered off with suction and dried under high vacuum.
Aufarbeitung
- stirringThe reaction solution is then stirred at room temperature for another two hours
- customThe phosphoryl chloride is removed under reduced pressure
- customa rotary evaporator
- additionWater/dichloromethane 9:1 is added to the residue, which
- waitis then boiled for 5 minutes
- filtrationthe product is filtered off with suction
- customdried under high vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-ed8e5fe2b94d43c7a773afc10623e42a
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07737153B2
Verknüpfte Notizen
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