反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 18 °C
PROCEDURE
实验过程
In a two-necked, round bottomed flask, equipped with a condenser and addition funnel, the 2-(dimethylamino)ethyl acetate (0.05 mol) was mixed with 30 mL of anhydrous hexane. Chloromethyl dodecyl ether (0.055 mol) was slowly added over 5 minutes. After 15 minutes, the reaction mixture was cooled to the temperature of minus 18° C. and the crude product was separated. The precipitate was washed with 30 mL of hexane and used in the next step without further purification. The crude (2-acetooxyethyl)-dodecyloxymethyldimethylammonium chloride was dissolved in 30 mL of water and aqueous solution of potassium benzoate (0.065 mol) was added. After 30 min, 30 mL of chloroform was added. The chloroform phase was separated and washed with distilled water until chloride ions were no longer detected using AgNO3. The obtained grease was dried under vacuum. The product was obtained as grease in 67% yield. Thermogravimetric analysis: Tonset=122° C. 1H and 13C NMR (DMSO) were obtained.
WORKUP
后处理
- customIn a two-necked, round bottomed flask, equipped with a condenser and addition funnel
- customthe crude product was separated
- washThe precipitate was washed with 30 mL of hexane
- customused in the next step without further purification
- dissolutionThe crude (2-acetooxyethyl)-dodecyloxymethyldimethylammonium chloride was dissolved in 30 mL of water
- waitAfter 30 min
- customThe chloroform phase was separated
- washwashed with distilled water until chloride ions
- customThe obtained grease was dried under vacuum
- customThe product was obtained as grease in 67% yield
- customTonset=122° C