反応 #809180

反応方程式

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

収率 98.6%

溶媒

water

反応条件

後処理

1. 1
   workup.ADDITIONSeparately, a 100 ml mixing vessel
2. 2
   workup.ADDITIONcontaining tube
3. 3
   その他Then the reaction of the mixture
4. 4
   workup.WAITwas carried out at a temperature of 50 to 55° C. for one hour
5. 5
   その他reaction liquid in the reaction vessel
6. 6
   その他the reaction liquid
7. 7
   その他The reaction liquid
8. 8
   抽出was subjected to an extraction procedure
9. 9
   抽出to extract the reaction product
10. 10
    抽出The resultant extraction liquid
11. 11
    濃縮was concentrated
12. 12
    その他evaporator

実験手順

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%).

出典