反应详情

温度

80 °C

A mixture of triclosan (29.0 g.), triethylamine (15 ml.) and 2,2-dimethylglutaric anhydride (20 g.) was heated at 80° C. for 5 hours. A further quantity (2.0 g.) of anhydride and triethylamine (1 ml.) were added and heating continued for 24 hours. The mixture was cooled to ambient temperature, washed with 2M hydrochloric acid (100 ml.), then with water (3×80 ml.) and dried (MgSO4). The solution obtained was evaporated. The brown residual oil was dissolved in hot cyclohexane. The solution on cooling gave white crystals which were recrystallised from cyclohexane/petrol 60-80 to give 5-chloro-2-(2,4-dichlorophenoxy)phenyl 4-carboxy-2,2-dimethylbutyrate (C') (12.7 g.), m.p. 125°-128° C.

1. temperatureheating
2. temperatureThe mixture was cooled to ambient temperature
3. washwashed with 2M hydrochloric acid (100 ml.)
4. dry with materialwith water (3×80 ml.) and dried (MgSO4)
5. customThe solution obtained
6. customwas evaporated
7. dissolutionThe brown residual oil was dissolved in hot cyclohexane
8. temperatureThe solution on cooling
9. customgave white crystals which
10. customwere recrystallised from cyclohexane/petrol 60-80