反应详情

温度

0 °C

About 100 g of the methoxymethoxybenzene manufactured in the synthesis example 1 and about 133.1 g of phenyl sulfoxide were mixed and stirred in about 1,200 ml of an MC, and then a temperature was reduced to about −78° C. using a dry ice-aceton. Next, about 240 g of trifluoromethanesulfonic anhydride was gradually dropped and stirred for about three hours using a dropping funnel at about −78° C. to perform a synthesis reaction (See Equation 2 below). Next, the synthesis reaction was terminated when an initiator on a thin layer chromatography (TLC) disappeared. Next, about 200 g of calcium carbonate was dissolved in about 1.5 L of water, and the reaction mixed liquid was added in a solvent cooled to about 0° C. and strongly stirred for about 20 minutes. Next, an organic phase was extracted, and further stirred in a calcium carbonate aqueous solution. Next, the extracted organic phase was washed using brine, and dried using magnesium sulphate. Next, the organic was filtered and concentrated to obtain about 200 g (a yield: about 58.5%) of a diphenyl-4-methoxymethoxyphenylsulfonium trifluoromethanesulfonate salt, and a structure of the diphenyl-4-methoxymethoxyphenylsulfonium trifluoromethanesulfonate salt was observed by 1H-NMR (See FIG. 2):

1. additionwere mixed
2. customwas reduced to about −78° C.
3. stirringstirred for about three hours
4. customat about −78° C.
5. customa synthesis reaction (
6. customNext, the synthesis reaction
7. customwas terminated when an initiator on a thin layer chromatography (TLC)
8. dissolutionNext, about 200 g of calcium carbonate was dissolved in about 1.5 L of water
9. additionthe reaction mixed liquid
10. additionwas added in a solvent
11. stirringstrongly stirred for about 20 minutes
12. extractionNext, an organic phase was extracted
13. stirringfurther stirred in a calcium carbonate aqueous solution
14. washNext, the extracted organic phase was washed
15. customdried
16. filtrationNext, the organic was filtered
17. concentrationconcentrated