反应详情

温度

60 °C

A 20-gallon jacketed stainless steel reactor equipped with a mechanical agitator is charged with 12.8 kg of ACN, 12.45 kg of DEK and 12.4 kg of 2-bromo-6-methoxynaphthalene (BMN) formed as described in Example 7 hereof, 4.6 g of PdCl2, and 50.9 g of NMDP. The reactor is pressured and vented three times with 50 psig nitrogen. The reactor is then charged with 6.27 kg of TEA. The agitator is set at 158 rpm and the reactor is pressured and vented with 50 psig nitrogen. The agitator is set to 416 rpm, the reactor is pressured to 100 psig with ethylene and heated with tempered water on the jacket. The reaction temperature ranges from 87° to 98° C., while the pressure varies from 394 to 458 psig. The total reaction time is 3.5 hours with a BMN conversion of 99.6% in two hours. The reactor is cooled, vented, and the reactor contents at 60° C. are transferred for workup, to a 30-gallon glass lined reactor equipped with a 6-inch column. The 20-gallon reactor is then charged with 12.5 kg of DEK, which is then heated to 60° C. and transferred to the 30-gallon reactor.

1. customequipped with a mechanical agitator
2. customformed
3. customranges from 87° to 98° C., while the pressure
4. temperatureThe reactor is cooled
5. customat 60° C.
6. customequipped with a 6-inch column
7. additionThe 20-gallon reactor is then charged with 12.5 kg of DEK, which