Sodium Hydroxide → HCID 67399735, Verbindung
Reaktionsgleichung
O.NN.[CH:4]1([C:7]2[CH:8]=[CH:9][C:10](/[C:15](/[C:30]3[CH:35]=[CH:34][C:33]([S:36][CH3:37])=[CH:32][CH:31]=3)=[CH:16]/[CH2:17][CH2:18][N:19]3C(=O)C4C(=CC=CC=4)C3=O)=[N:11][C:12]=2[O:13][CH3:14])[CH2:6][CH2:5]1.[OH-].[Na+]>C(O)C>[CH:4]1([C:7]2[CH:8]=[CH:9][C:10](/[C:15](/[C:30]3[CH:35]=[CH:34][C:33]([S:36][CH3:37])=[CH:32][CH:31]=3)=[CH:16]/[CH2:17][CH2:18][NH2:19])=[N:11][C:12]=2[O:13][CH3:14])[CH2:6][CH2:5]1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 95 °C
Versuchsvorschrift
Hydrazine monohydrate (1 mL) was added to a solution of 2-{(3E)-4-(5-cyclopropyl-6-methoxypyridin-2-yl)-4-[4-(methylsulfanyl)phenyl]but-3-en-1-yl}-1H-isoindole-1,3(2H)-dione (320 mg) in ethanol (4 mL), and the mixture was stirred at 95° C. for one hour. The reaction solution was poured into a 3 M sodium hydroxide solution, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure to give (3E)-4-(5-cyclopropyl-6-methoxypyridin-2-yl)-4-[4-(methylsulfanyl)phenyl]but-3-en-1-amine as a colorless amorphous (225 mg, 97%).
Aufarbeitung
- extractionfollowed by extraction with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customafter which the solvent was evaporated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-dbf7988bd3ec4d628f3d942f5381f4fb
- Quelldatensatz
- uspto-grants-2014_09
- Patentnummer
- US08822503B2
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