反应详情

1-Chloro-4-hydroxythioxanthone as prepared in Example 1 (6.6 g), potassium carbonate (4.1 g), 2-butanone (60 ml) and water (6 ml) were heated under reflux. Benzoyl chloride (5.3 g) was added over 20 minutes and the mixture heated under reflux for 3 hours. A solid precipitated from solution during the heating period. The mixture was cooled, quenched with water (120 ml), the solid filtered and recrystallised from 2-butanone with a charcoal treatment. The title compound (6.8 g; 74.0%) was obtained of mp 177°-78°. Analysis C20H11ClO3S=366.81 Requires C 65.48% H 3.02% Cl 9.67% S 8.74% Found C 65.46% H 3.13% Cl 9.77% S 8.70%

1. temperaturewere heated
2. temperatureunder reflux
3. temperaturethe mixture heated
4. temperatureunder reflux for 3 hours
5. customA solid precipitated from solution during the heating period
6. temperatureThe mixture was cooled
7. customquenched with water (120 ml)
8. filtrationthe solid filtered
9. customrecrystallised from 2-butanone with a charcoal treatment