反应详情

温度

0 °C

10 g (0.04 mol) of methyl 5,8-dimethyl-4-hydroxy-6-thiochromanecarboxylate and 4.9 g (0.06 mol) of sodium acetate were together added to 200 ml of methanol. The mixture was cooled to 0° C. and slowly admixed with a solution of 41.4 g (0.07 mol) of OXONE® (potassium peroxymonosulfate) in 200 ml of water. During the addition, the reaction temperature was kept below 6° C. The mixture was subsequently stirred at room temperature for 4 h and then diluted with 120 ml of water. The mixture was extracted with methylene chloride (3×200 ml), and the extract was dried over MgSO4 and concentrated using a rotary evaporator.

1. additionDuring the addition
2. customwas kept below 6° C
3. extractionThe mixture was extracted with methylene chloride (3×200 ml)
4. dry with materialthe extract was dried over MgSO4
5. concentrationconcentrated
6. customa rotary evaporator