反应详情

温度

0 °C

3,4-(Dimethylmethylenedioxy)-5-hexene-1,2-diol (9.77 g) was mixed with 155 ml of pyridine and 52 ml of chloroform, and 11.39 g of p-toluenesulfonyl chloride was added gradually in four portions at 0° C. The mixture was stirred at 0° C. for 6 hours, poured into 6N hydrochloric acid with ice and extracted with diethyl ether. The extract was washed with a saturated sodium hydrogen carbonate aqueous solution and a saturated sodium chloride aqueous solution in sequence, dried with anhydrous ride aqueous solution in sequence, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure to afford 17.88 g of 3,4-(dimethylmethylenedioxy)-2-hydroxy-5-hexen-1-yl p-toluenesulfonate having the following properties.

1. additionwas added gradually in four portions at 0° C
2. extractionextracted with diethyl ether
3. washThe extract was washed with a saturated sodium hydrogen carbonate aqueous solution
4. dry with materiala saturated sodium chloride aqueous solution in sequence, dried with anhydrous ride aqueous solution in sequence
5. dry with materialdried with anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure