Reaktionsgleichung
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[C:13]([N+:15]([O-:17])=[O:16])[CH:12]=[CH:11][C:10]=2[CH3:18])[CH:3]=1.OB(O)[C:21]1[CH:22]=[N:23][CH:24]=[N:25][CH:26]=1>C(O)C>[CH3:18][C:10]1[CH:11]=[CH:12][C:13]([N+:15]([O-:17])=[O:16])=[CH:14][C:9]=1[NH:8][C:4]1[CH:3]=[C:2]([C:21]2[CH:22]=[N:23][CH:24]=[N:25][CH:26]=2)[N:7]=[CH:6][N:5]=1Komponenten
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
3.28 g of 2-[(6-chloro)pyrimidin-4-ylamino]-1-methyl-4-nitrobenzene (Reference Example 20 (step 1)) were dissolved with heating in 130 ml of anhydrous ethanol. 1.69 g of dihydroxy(5-pyrimidinyl)borane was added, and then deaeration was performed, followed by purging with argon. 5.82 g of potassium carbonate and 2.15 g of tetrakis(triphenylphosphine)palladium (0) were added in turn, and then the mixture was heated at reflux for 7.5 hours. The reaction solution was mixed with water, followed by extraction with ethyl acetate twice, and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was crystallized by adding chloroform-methanol to obtain 808 mg of the objective compound as ocherous crystals.
Aufarbeitung
- customby purging with argon
- addition5.82 g of potassium carbonate and 2.15 g of tetrakis(triphenylphosphine)palladium (0) were added in turn
- temperaturethe mixture was heated
- temperatureat reflux for 7.5 hours
- additionThe reaction solution was mixed with water
- extractionfollowed by extraction with ethyl acetate twice
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was crystallized
- additionby adding chloroform-methanol
Quellen und Nachweise
- ORD-Eintrag
- ord-a64403ea725c4d388b7aaeea14906f45
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07728131B2
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