反应详情

温度

6.5 °C

Sodium azide (160 kg) was dissolved in pure water (505 L), and the solution was cooled to 3 to 10° C. Trioctyltin chloride [TOTC] (847 kg) was added dropwise over 1 to 3 hours, followed by stirring at 5 to 10° C. for about 2 hours. The reaction solution was extracted with methylene chloride (1822 kg, then 546 kg). The methylene chloride layer was washed with a mixture of pure water (50 L) and a 10% aqueous sodium chloride solution (440 L), and the methylene chloride layer was concentrated under reduced pressure to give trioctyltin azide [TOTA].

1. extractionThe reaction solution was extracted with methylene chloride (1822 kg
2. washThe methylene chloride layer was washed with a mixture of pure water (50 L)
3. concentrationa 10% aqueous sodium chloride solution (440 L), and the methylene chloride layer was concentrated under reduced pressure