反应详情

温度

110 °C

A ten weight percent (10 wt. %) solution of n-butylethylmagnesium (BEM) in n-heptane was prepared as follows. A pressure bottle was prepared and heated in an oil bath thermostatically controlled at 115° C. The pressure bottle was equipped with a stirrer. Magnesium powder (18.0 grams, 0.0740 mole) was charged to the pressure bottle and allowed to heat at about 110° C. under a purge of nitrogen. The bottle was removed from the bath and 200 grams (g) dry n-heptane was added. A small amount (0.2 g) of triethylaluminum was injected into the heptane under nitrogen atmosphere to serve as an activator and viscosity reducer. After the pressure bottle was established as the bath temperature, a mixture of ethyl chloride (23.9 g, 0.370 mole) and n-butyl chloride (34.2 g, 0.369 mole) was slowly charged. Temperature was held at 115°-120° C. The addition took 1.5 hours; the pressure rose to about 35 psig. Some 30 minutes was allowed for completion of the reaction, and the slurry was allowed to settle while cooling. Analysis of the clear liquid gave the following results: Mg, 2.82 wt. %; Al, 0.02 wt. %; Cl, 0.11 wt. %. Analysis of the hydrolysis gas gave a composition of 50.9 mole percent n-butane and 49.1 mole % ethane.

1. customA pressure bottle was prepared
2. temperatureheated in an oil bath
3. customthermostatically controlled at 115° C
4. customThe pressure bottle was equipped with a stirrer
5. customa purge of nitrogen
6. customThe bottle was removed from the bath and 200 grams (g) dry n-heptane
7. additionwas added
8. additionwas slowly charged
9. customwas held at 115°-120° C
10. additionThe addition
11. customSome 30 minutes was allowed for completion of the reaction
12. temperaturewhile cooling
13. customAnalysis of the clear liquid gave the
14. customfollowing results
15. customAnalysis of the hydrolysis gas