反应详情

温度

125 °C

1,5-Dichloroanthraquinone (100 parts) is added at room temperature with stirring to a mixture of dimethylformamide (474 parts), thiophenol (135 parts) and potassium carbonate (63 parts). The suspension is heated at 125° C. for 3 hours, cooled to room temperature and then cooled to 5° C. for 1 hour. The precipitate is filtered off and washed with a 50/50 mixture of 95% ethanol and 8% sodium hydroxide solution (2×250 parts). The filter cake is then slurried with a further 500 parts of the ethanol/sodium hydroxide solution mixture. After stirring at room temperature for 1 hour, the precipitate is filtered off and washed again with ethanol/sodium hydroxide solution mixture (5×100 parts), followed by water (250 parts) containing glacial acetic acetic acid (25 parts) and finally water (3×250 parts). The filter-cake is dried at 70° C. giving 140.4 parts of 1,5-bis(phenylthio) anthraquinone, mp (melting point) 256° C.

1. temperaturecooled to room temperature
2. temperaturecooled to 5° C. for 1 hour
3. filtrationThe precipitate is filtered off
4. washwashed with a 50/50 mixture of 95% ethanol and 8% sodium hydroxide solution (2×250 parts)
5. filtrationthe precipitate is filtered off
6. washwashed again with ethanol/sodium hydroxide solution mixture (5×100 parts)
7. additioncontaining glacial acetic acetic acid (25 parts) and finally water (3×250 parts)
8. customThe filter-cake is dried at 70° C.