反应详情

温度

20 °C

L-Rhamnose monohydrate (168.3 g, 0.92 mol) is added as a solid in portions, under strong stirring, to a mixture of 1,3-propanedithiol (100 g, 0.92 mol) in 500 ml of 37% HCl. The resulting solution is kept under stirring for 12 hours at about 20° C. Already at the first hour, formation of an abundant white precipitate is observed. The suspension is then cooled to 5-10° C. and the acid excess is neutralized with NaOH and 500 ml of ice. The suspension at pH of about 7 is then filtered and the solid is washed with water and 100 ml of isopropanol. The wet solid is dried under vacuum at 40° C. for 16 hours to attain 222 g of product (XII) as an off-white solid in 95% yield.

1. temperatureThe suspension is then cooled to 5-10° C.
2. filtrationThe suspension at pH of about 7 is then filtered
3. washthe solid is washed with water and 100 ml of isopropanol
4. customThe wet solid is dried under vacuum at 40° C. for 16 hours