反应详情

温度

125 °C

A reactor equipped with stirrer, reflux condenser, dropping funnel and thermometer is charged with 130.23 g (1.0 mol) of isooctanol (mixture of isomers), 3.14 g (0.02 mol) of powdered tin difluoride and 5.28 g (0.02 mol) of 18-crown-6 (crown ether) and the charge is heated to 125° C. The, with efficient stirring, 86.26 ml (1.1 mol) of epichlorohydrin are added over 30 minutes. The reaction is allowed to continue for 20 hours, during which time the temperature rises to about 130° C. The reaction mixture is cooled to 55° C. and then, at this temperature, 88 g (1.1 mol) of a 50% aqueous solution of sodium hydroxide are added dropwise with efficient stirring over 30 minutes. After stirring for 6 hours at 55°-60° C. and cooling to room temperature, the suspension is filtered and the filtrate is washed with ethyl acetate. The phases are separated, and the aqueous phase is extracted with 2×100 ml of ethyl acetate. The combined organic phases are washed with as small an amount of 10% KH2PO4 solution as possible and then with water until neutral, dried over magnesium sulfate and filtered. The filtrate is freed from solvent on a rotary evaporator under vacuum (bath temperature 50° C.). Yield: 180.7 g (97% of theory) of colourless isooctanol glycidyl ether (mixture of isomers) for which the following analytical values are obtained: epoxy value: 4.71 eq/kg (88% of theory); total chlorine content: 2.7%; hydrolysable chlorine content: 122 ppm.

1. customA reactor equipped with stirrer
2. temperaturereflux condenser
3. customrises to about 130° C
4. temperatureThe reaction mixture is cooled to 55° C.
5. stirringAfter stirring for 6 hours at 55°-60° C.
6. temperaturecooling to room temperature
7. filtrationthe suspension is filtered
8. washthe filtrate is washed with ethyl acetate
9. customThe phases are separated
10. extractionthe aqueous phase is extracted with 2×100 ml of ethyl acetate
11. washThe combined organic phases are washed with as small an amount of 10% KH2PO4 solution as possible and then with water until neutral,
12. dry with materialdried over magnesium sulfate
13. filtrationfiltered
14. customThe filtrate is freed from solvent on a rotary evaporator under vacuum (bath temperature 50° C.)