反应详情

In the apparatus described under Example 1, 21.8 g of reactant A (0.2 mol), 25.8 g of p-trichloromethyl-benzoyl chloride (0.1 mol) and 3.5 g of B2O3 (0.05 mol) were mixed and slowly heated. Between 190° and 200° C, a vigorous evolution of HCl began. After 2 hours the mixture was cooled and ground in a mortar. After extraction twice with 100 ml of CHCl3 and twice with 100 ml of water, 22.3 g of raw product (71% of the theory) was obtained, melting at 318° to 328° C. Compound XIX can be recrystallized from dimethylformamide, o-dichlorobenzene, nitrobenzene, dimethylsulfoxide or 1,2-dibromoethane. A small specimen recrystallized from o-dichlorobenzene melted at 325° to 329° C. The product can be further purified by chromatography on Al2O3 with 1,2-dibromoethane as the elutant at 120° C, whereupon the melting point becomes 340° to 342° C.

1. additionwere mixed
2. temperatureslowly heated
3. customBetween 190°
4. custom200° C
5. temperatureAfter 2 hours the mixture was cooled
6. extractionAfter extraction twice with 100 ml of CHCl3