反应详情

A 4 N aqueous solution of sodium hydroxide (150 cc) is added, at a maximum of 20° C., to a suspension of 4-hydroxy-3-(pyrid-2-yl)-thiazolidine-2-thione (127.5 g) in methanol (900 cc), and a solution of potassium borohydride (33.0 g) in water (150 cc) is then added at a maximum of 20° C. The reaction is allowed to proceed for 1 hour at 20° C. A 4 N aqueous solution of hydrochloric acid (300 cc) is added at a maximum of 20° C. The methanol is evaporated off under reduced pressure (20 mm Hg) at 45° C. The aqueous phase is extracted 3 times with methylene chloride (2.5 liters in total). The organic solution is washed 3 times with distilled water (1.5 liters in total), dried over sodium sulphate and evaporated. The resulting product (110.0 g) is purified by recrystallisation from a mixture of acetonitrile (100 cc) and isopropyl ether (200 cc). After drying under reduced pressure (0.2 mm Hg) at 40° C., 2-hydroxyethyl pyrid-2-yldithiocarbamate (85.1 g), which melts at 88° C., is obtained.

1. customThe methanol is evaporated off under reduced pressure (20 mm Hg) at 45° C
2. extractionThe aqueous phase is extracted 3 times with methylene chloride (2.5 liters in total)
3. washThe organic solution is washed 3 times with distilled water (1.5 liters in total)
4. dry with materialdried over sodium sulphate
5. customevaporated
6. customThe resulting product (110.0 g) is purified by recrystallisation from a mixture of acetonitrile (100 cc) and isopropyl ether (200 cc)
7. customAfter drying under reduced pressure (0.2 mm Hg) at 40° C.