반응 #809180

반응 방정식

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

수율 98.6%

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONSeparately, a 100 ml mixing vessel
2. 2
   workup.ADDITIONcontaining tube
3. 3
   기타Then the reaction of the mixture
4. 4
   workup.WAITwas carried out at a temperature of 50 to 55° C. for one hour
5. 5
   기타reaction liquid in the reaction vessel
6. 6
   기타the reaction liquid
7. 7
   기타The reaction liquid
8. 8
   추출was subjected to an extraction procedure
9. 9
   추출to extract the reaction product
10. 10
    추출The resultant extraction liquid
11. 11
    농축was concentrated
12. 12
    기타evaporator

실험 절차

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%).

출처