反应详情

温度

70 °C

3.5 g of methyl 4-(4-chlorosulfonyl-3-pentafluorosulfanylphenoxy)-5-methanesulfonyl-2-methylbenzoate were added in portions to a solution of 8.10 g of Na2SO3 in 75 ml of water at 70° C., during which the pH was kept at about pH=10 with 10 molar aqueous NaOH solution. The mixture is then stirred at 70° C. for 45 minutes and, after being allowed to cool, the pH is adjusted to pH=2 with aqueous HCl solution. 3 extractions with 200 ml of EA each time were carried out. After drying over MgSO4, the solvent was removed in vacuo. The residue was suspended in 100 ml of water and adjusted to pH=10 with a 2 molar aqueous NaOH solution, and the volatiles were removed in vacuo. Coevaporation was then carried out firstly twice with 100 ml of toluene each time and then with 100 ml of anhydrous DMF, and the residue (3.0 g) was reacted further without purification.

1. temperatureto cool
2. extraction3 extractions with 200 ml of EA each time
3. dry with materialAfter drying over MgSO4
4. customthe solvent was removed in vacuo
5. customthe volatiles were removed in vacuo
6. customwith 100 ml of anhydrous DMF, and the residue (3.0 g) was reacted further without purification