Reaktionsgleichung
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[NH:8][CH:9]=[CH:10][C:3]=12.[F:11][C:12]1[CH:13]=[C:14]([CH:16]=[CH:17][C:18]=1[OH:19])[NH2:15].[OH-].[K+]>O>[F:11][C:12]1[CH:13]=[C:14]([CH:16]=[CH:17][C:18]=1[O:19][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[NH:8][CH:9]=[CH:10][C:3]=12)[NH2:15]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
543 mg (3.56 mmol) of 4-chloro-1H-pyrrolo[2,3-b]pyridine (from example XVIII, 905 mg (7.12 mmol) of 3-fluoro-4-hydroxyaniline and 399 mg (7.12 mmol) of powdered potassium hydroxide are heated at 260° C. for 8 hours. Another 905 mg (7.12 mmol) of 3-fluoro-4-hydroxyaniline and 200 mg (3.56 mmol) of powdered potassium hydroxide are added, and the mixture is reacted at 260° C. for another 8 h. For work-up, the mixture is cooled to room temperature, diluted with water and extracted three times with ethyl acetate. The organic phase is dried over magnesium sulfate and concentrated using a rotary evaporator. The residue is purified by preparative HPLC. The fractions which, according to LC-MS, contain 39% of product are used without further purification for the next reaction.
Aufarbeitung
- customthe mixture is reacted at 260° C. for another 8 h
- extractionextracted three times with ethyl acetate
- dry with materialThe organic phase is dried over magnesium sulfate
- concentrationconcentrated
- customa rotary evaporator
- customThe residue is purified by preparative HPLC
- customare used without further purification for the next reaction
Quellen und Nachweise
- ORD-Eintrag
- ord-e1ae06632b2441b793d7925135e5427b
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07737153B2
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