Reaktion #575094
ord-6295631e3f164ff297119d6e328a365f
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONthat addition
- 2workup.WAITAfter a further hour at 0° C.
- 3SonstigeThe precipitate was separated off
- 4Waschenwashed with water until neutral and
- 5Sonstigedried
Vorschrift
A solution of 7.4 g (66 mmol) of potassium tert-butylate in 50 ml of tert-butanol was added dropwise to a vigorously stirred mixture of 8.0 g (33 mmol) of 2-amino-4-(2,4-dichlorophenyl)thiazole, 9.8 g (37 mmol) of 2,4-dinitro-6-trifluoromethylchlorobenzene and 100 ml of tetrahydrofuran/tert-butanol (1:2) at 0° to 5° C. in such a way that addition was complete after 1 hour. After a further hour at 0° C., the mixture was slowly warmed, over the course of about 2 hours, to 20° C. The mixture was then adjusted to pH 4 with glacial acetic acid and diluted with about 1 l of water. The precipitate was separated off, washed with water until neutral and dried. Yield: 90%; melting point 125° to 130° C.