反应详情

温度

330 °C

A 1-1 V2A stainless steel vessel equipped with a horseshoe stirrer was charged with 600 g of potassium hydroxide and 60 g of sodium carbonate, and 250 g of the crude product described under (a) were added at 300° C a little at a time over 2 hours. The temperature was raised to 330° C, and the contents were stirred for 3 hours. The contents were then cooled down in a controlled manner by addition of water, diluted with a total of 1.6 1 of water and filtered with suction. The residue was suspended in 2 l of water, and the suspension was acidified with concentrated hydrochloric acid, heated to 90° C and filtered with suction while still hot. The residue was dried and recrystallized from N,N-dimethylformamide. Purity (HPLC) 99.8%; yield: 102.0 g (74% based on terphenyl).

1. additionwere added at 300° C a little at a time over 2 hours
2. filtrationfiltered with suction
3. temperatureheated to 90° C
4. filtrationfiltered with suction while still hot
5. customThe residue was dried
6. customrecrystallized from N,N-dimethylformamide