反应 #2200576

反应方程式

sodium carbonate

N,N,3,3-tetramethylbutylamine

1-bromo-3,3-dimethylbutane

isopropanol

→

N,N-dimethyl-N,N-di(3,3-dimethylbutyl)ammonium bromide

溶剂

diethyl ether

反应条件

后处理

1. 1
   其他is prepared
2. 2
   workup.WAITA white solid appears, and after this period
3. 3
   温度to increase the amount of precipitate
4. 4
   其他The isopropanol and the diethyl ether are then evaporated at 30° C. by means of a rotary evaporator
5. 5
   其他The organic product that is formed
6. 6
   萃取is extracted from the reaction mixture by means of dichloromethane
7. 7
   萃取Three successive extractions with 10 ml of dichloromethane
8. 8
   其他The organic phase that is obtained
9. 9
   其他is evaporated by means of a rotary evaporator
10. 10
    其他The white solid that is formed
11. 11
    洗涤is washed with dry diethyl ether
12. 12
    过滤filtered on a nylon membrane (Ø=0.2 μm)

实验过程

A mixture that contains 1 g (0.77.10−2 mol) of N,N,3,3-tetramethylbutylamine (Aldrich) and 1.917 g (1.16.10−2 mol) of 1-bromo-3,3-dimethylbutane (Prolabo) and about 4 ml of isopropanol is prepared. 1.23 g (1.16.10−2 mol) of sodium carbonate is then added. This suspension is brought to reflux for 2 days at the temperature of 100° C. A white solid appears, and after this period, about 5 ml of diethyl ether is added to the reaction mixture so as to increase the amount of precipitate. The isopropanol and the diethyl ether are then evaporated at 30° C. by means of a rotary evaporator. The organic product that is formed is extracted from the reaction mixture by means of dichloromethane. Three successive extractions with 10 ml of dichloromethane are carried out. The organic phase that is obtained is evaporated by means of a rotary evaporator. The white solid that is formed is washed with dry diethyl ether and filtered on a nylon membrane (Ø=0.2 μm). 0.8 g (0.27.10−2 mol) of N,N-dimethyl-N,N-di(3,3-dimethylbutyl)ammonium bromide (DMDMBA-Br) is then obtained. The nature of the radical that is obtained was verified by nuclear magnetic resonance of the proton; the results of this analysis are provided below. NMR 1H (D2O, 400 MHz, 25° C., δ ppm /TMS): 0.83 (s, 18H), 1.51-1.55 (m, 4H), 2.91 (s, 6H), 3.18-3.23 (m, 4H).

来源