Reacción #809180

Ecuación de reacción

calcium chloride

sulfuric acid

1,2-epoxydodecane

1,2-epoxydodecane

1,3-butanediol

sodium hydrogen carbonate

1,2-epoxydodecane

1,2-epoxydodecane

→

1,3-butanediol monohydroxydodecyl ether

Rendimiento 98.6%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONSeparately, a 100 ml mixing vessel
2. 2
   workup.ADDITIONcontaining tube
3. 3
   OtroThen the reaction of the mixture
4. 4
   workup.WAITwas carried out at a temperature of 50 to 55° C. for one hour
5. 5
   Otroreaction liquid in the reaction vessel
6. 6
   Otrothe reaction liquid
7. 7
   OtroThe reaction liquid
8. 8
   Extracciónwas subjected to an extraction procedure
9. 9
   Extracciónto extract the reaction product
10. 10
    ExtracciónThe resultant extraction liquid
11. 11
    Concentraciónwas concentrated
12. 12
    Otroevaporator

Procedimiento

Separately, a 100 ml mixing vessel equipped with a calcium chloride-containing tube was charged with 36.9 g (0.20 mole) of 1,2-epoxydodecane. While the charged 1,2-epoxydodecane was stirred and cooled with water, a concentrated sulfuric acid was gradually dropped in an amount of 0.4 g (0.004 mole) into the cooled 1,2-epoxydodecane. After stirring for 15 minutes, the resultant mixture was placed into the dropping apparatus attached to the reaction vessel and was dropped into 1,3-butanediol contained in the reaction vessel and maintained at a temperature of 50 to 55° C. over a time of 2 hours. Then the reaction of the mixture was carried out at a temperature of 50 to 55° C. for one hour. After the exhaustion of the starting material, namely 1,2-epoxydodecane was confirmed by a thin-layer chromatography, the reaction was stopped. A saturated aqueous sodium hydrogen carbonate solution was mixed in an amount of 50 ml into the resultant reaction liquid in the reaction vessel, the resultant mixture was stirred for 10 minutes to neutralize the reaction liquid. The reaction liquid was subjected to an extraction procedure using diethyl ether to extract the reaction product. The resultant extraction liquid was concentrated by using rotary evaporator. A 1,3-butanediol monohydroxydodecyl ether mixture was obtained in an amount of 52.8 g (yield: 98.6%).

Fuente