反应详情

A 20-gallon jacketed stainless steel reactor equipped with a mechanical agitator is charged with 19.45 kg of acetonitrile (ACN) and 12.45 kg of 2-bromo-6-methoxynaphthalene (BMN) formed as described in Example 7 hereof, and 4.8 g of PdCl2. The reactor is pressured and vented three times with 50 psig nitrogen. The reactor is then charged with 5.3 kg of ACN and 5.64 kg of triethylamine (TEA). The agitator is set at 158 rpm and the reactor is pressured and vented three times with 80 psig nitrogen. The reactor is then purged for ten minutes with nitrogen. Next a mixture of 48.6 g of neomenthyldiphenylphosphine (NMDP) dissolved in 0.35 kg of TEA is charged to the reactor. The agitator is set to 412 rpm and the reactor is heated with steam on the jacket. The reaction temperature is initially in the range of 91°-109° C., while the pressure varies from 412°-519 psig. The reaction produces a heat kick, and after 30 minutes the temperature rises to 109° C. with 26° C. cooling water on the jacket. The total reaction time is 1.75 hours with a BMN conversion of 100%. The reactor is cooled, vented, and the reactor contents are transferred to a 30-gallon glass lined reactor for workup.

1. customequipped with a mechanical agitator
2. customformed
3. customThe reactor is then purged for ten minutes with nitrogen
4. additionNext a mixture of 48.6 g of neomenthyldiphenylphosphine (NMDP)
5. dissolutiondissolved in 0.35 kg of TEA
6. additionis charged to the reactor
7. temperaturethe reactor is heated with steam on the jacket
8. customis initially in the range of 91°-109° C., while the pressure
9. customThe reaction produces a heat kick
10. temperatureThe reactor is cooled