反应详情

温度

2 °C

1-Bromo-3,3-dimethylbutan-2-one (40.0 g) is added to a suspension of triethylammonium (6-methylpyrid-2-yl)dithiocarbamate (64.0 g) in anhydrous acetonitrile (600 cc) at a maximum temperature of 20° C. The reaction is continued for 2 hours at 20° C. The insoluble hydrobromide of triethylamine is removed by filtration and washed with acetonitrile (50 cc). The organic phases are combined and evaporated under reduced pressure (20 mm.Hg) at 45° C. The residual oil is treated with diethyl ether (1200 cc). After 1 hour at 20° C., the ethereal solution is filtered, washed twice with distilled water (total 400 cc), dried over sodium sulphate and evaporated. The product obtained (60.0 g) is dissolved in boiling diisopropyl ether (870 cc) and the boiling solution is filtered. After 1 hour's cooling at 2° C., the resulting crystals are filtered off, washed twice with ice-cold diisopropyl ether (total 100 cc) and dried under reduced pressure (0.1 mm.Hg) at 40° C. to give 3,3-dimethyl-2-oxobutyl (6-methylpyrid-2-yl)dithiocarbamate (44.1 g) melting at 80° C.

1. customThe insoluble hydrobromide of triethylamine is removed by filtration
2. washwashed with acetonitrile (50 cc)
3. customevaporated under reduced pressure (20 mm.Hg) at 45° C
4. additionThe residual oil is treated with diethyl ether (1200 cc)
5. waitAfter 1 hour at 20° C.
6. filtrationthe ethereal solution is filtered
7. washwashed twice with distilled water (total 400 cc)
8. dry with materialdried over sodium sulphate
9. customevaporated
10. customThe product obtained (60.0 g)
11. dissolutionis dissolved
12. filtrationthe boiling solution is filtered
13. filtrationthe resulting crystals are filtered off
14. washwashed twice with ice-cold diisopropyl ether (total 100 cc)
15. customdried under reduced pressure (0.1 mm.Hg) at 40° C.