反应详情

温度

70 °C

3.5 g of methyl 4-(4-chlorosulfonyl-3-pentafluorosulfanylphenoxy)-5-methanesulfonyl-2-methylbenzoate (example 3) were added in portions to a solution, at 70° C., of 8.10 g of Na2SO3 in 75 ml of water and kept at about pH=10 with 10 molar aqueous NaOH solution. Subsequently, the mixture was stirred at 70° C. for 45 minutes, then allowed to cool and adjusted to pH=2 with aqueous HCl solution. The mixture was extracted 3 times with 200 ml each time of EA. The mixture was dried over MgSO4 and the solvent was removed under reduced pressure. The residue was suspended in 100 ml of water and adjusted to pH=10 with a 2 molar aqueous NaOH solution, and the volatile constituents were removed under reduced pressure. The mixture was subsequently extracted twice with 100 ml each time of toluene and then coevaporated with 100 ml of anhydrous DMF, and the residue (3.0 g) was reacted further without purification.

1. temperatureto cool
2. extractionThe mixture was extracted 3 times with 200 ml each time of EA
3. dry with materialThe mixture was dried over MgSO4
4. customthe solvent was removed under reduced pressure
5. customthe volatile constituents were removed under reduced pressure
6. extractionThe mixture was subsequently extracted twice with 100 ml each time of toluene
7. customthe residue (3.0 g) was reacted further without purification