反应详情

温度

40 °C

In a reactor 68 kg dichloromethane, 20 kg 5-nitro-vanillic acid of example 1b, 76 gram of N,N-dimethylformamide and 13.4 kg (8 L) thionyl chloride, was charged at 20.2° C. The mixture was heated to 40° C. until all the starting material dissolved and the evolution of HCl and SO2 stopped. When all the starting material was consumed 5-10 L dichloromethane was distilled off at normal pressure at 40° C. then the mixture was cooled to 20-25° C. and the distillation was continued until dry under vacuum at 40° C. The evaporation residue was dissolved in 36 kg dry THF. The THF solution was used in Example 4d.

1. dissolutiondissolved
2. customWhen all the starting material was consumed 5-10 L dichloromethane
3. distillationwas distilled off at normal pressure at 40° C.
4. temperaturethe mixture was cooled to 20-25° C.
5. distillationthe distillation
6. customuntil dry under vacuum at 40° C
7. dissolutionThe evaporation residue was dissolved in 36 kg dry THF