反应详情

温度

45 °C

3.0 g of sodium 4-(2-methanesulfonyl-4-methoxycarbonyl-5-methyl-phenoxy)-2-pentafluorosulfanylbenzenesulfinate (example 4) were dissolved in 100 ml of anhydrous DMF, 4.0 g of CH31 were added and the mixture was stirred at 45° C. for 9 h. The reaction mixture was subsequently left to stand at RT for 2 days. The solvent was then removed under reduced pressure and the residue taken up with 100 ml of water and 100 ml of EA. 50 ml of a 5% aqueous NaHSO4 solution were then added and the phases were separated. Subsequently, the mixture was extracted 3 times with 100 ml each time of EA. The mixture was dried over MgSO4, the solvent was removed under reduced pressure and the residue was chromatographed on silica gel with 1:1 MTB/DIP. 0.59 g of methyl 5-methanesulfonyl-4-(4-methanesulfonyl-3-pentafluorosulfanylphenoxy)-2-methylbenzoate and 0.49 g of methyl 5-methanesulfonyl-4-(4-methoxysulfinyl-3-pentafluorosulfanylphenoxy)-2-methylbenzoate were obtained.

1. addition4.0 g of CH31 were added
2. waitThe reaction mixture was subsequently left
3. waitto stand at RT for 2 days
4. customThe solvent was then removed under reduced pressure
5. addition50 ml of a 5% aqueous NaHSO4 solution were then added
6. customthe phases were separated
7. extractionSubsequently, the mixture was extracted 3 times with 100 ml each time of EA
8. dry with materialThe mixture was dried over MgSO4
9. customthe solvent was removed under reduced pressure
10. customthe residue was chromatographed on silica gel with 1:1 MTB/DIP