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cmj-nankai鐵桿木蟲 (小有名氣)
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鐵桿木蟲 (著名寫手)
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Preperation of sulfonium gel The most part of sulfonium gels have been obtained by alkylation of sulfides (or of thiols) with the alcohol (or the ether) in acidic medium. Salt of alkyl diphenyl sulfonium. The preparation of salt of alkyl-(saturated) diphenyl sulfonium have been described recently. Triflate of diphenyphenylsulfonium. At 3.7 ml (0.2mol) anhydrous Ph2S in 200ml pentane and 10ml of CH2Cl2 containing 10ml (0.1mol) phenol cooled to -40C and under argon, we add 16.8ml trifluoromethanesulfonic anhydride. After 16h at -40C, we stop the agitation. The solvent is canceled and the solid washed in pentane, and then dissolved in a CH2Cl-Et2O mixture and finally cooled to -78C for several hours. The solid who has precipitated is stripped from solvent and dried at -40C under 10-3mmHg during 5 h. We obtained approximate 20g (50%) of crystals very unstable. NMR….. |
2樓2015-04-10 20:02:43
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