反应详情

温度

2 °C

A 50% (by weight) aqueous solution of chloroacetaldehyde (28.4 g) is added, at a maximum temperature of 30° C., to a solution of triethylammonium (6-methylpyrid-2-yl)-dithiocarbamate (51.5 g) in distilled water (225 cc). The reaction is continued for 2 hours at 20°-30° C. The resulting crystals are separated by filtration, washed five times with distilled water (total 125 cc) and dried in air at 20° C. The product obtained (37.0 g; m.p. 127° C.) is dissolved in a mixture of chloroform (600 cc) and diethyl ether (300 cc); the organic solution is washed three times with distilled water (total 450 cc), dried over sodium sulphate, treated with decolorising charcoal (1 g) and evaporated. The crystals obtained (34.0 g; m.p. 128° C.) are dissolved in boiling ethanol (240 cc). After 2 hours cooling at 2° C., the resulting crystals are separated by filtration, washed twice with ice-cold ethanol (total 30 cc) and dried under reduced pressure (0.1 mm.Hg) at 50° C. 4-Hydroxy-3-(6-methylpyrid-2-yl)-thiazolidine-2-thione (28.8 g), melting at 128° C., is thus obtained.

1. customThe resulting crystals are separated by filtration
2. washwashed five times with distilled water (total 125 cc)
3. customdried in air at 20° C
4. customThe product obtained (37.0 g; m.p. 127° C.)
5. washthe organic solution is washed three times with distilled water (total 450 cc)
6. dry with materialdried over sodium sulphate
7. additiontreated with decolorising charcoal (1 g)
8. customevaporated
9. customThe crystals obtained (34.0 g; m.p. 128° C.)
10. dissolutionare dissolved
11. customthe resulting crystals are separated by filtration
12. washwashed twice with ice-cold ethanol (total 30 cc)
13. customdried under reduced pressure (0.1 mm.Hg) at 50° C