反应详情

温度

20 °C

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.

1. additionthat addition
2. waitAfter a further hour at 0° C.
3. customThe precipitate was separated off
4. washwashed with water until neutral and
5. customdried