反应详情

温度

73 °C

A 10 N aqueous solution of sodium hydroxide (100 cc) is added dropwise, in the course of 20 minutes and whilst keeping the temperature below 15° C., to a solution of 2-(pyrid-2-ylmethyl)-isothiourea dihydrochloride (120 g) in distilled water (250 cc), cooled to 13° C. After heating for 20 minutes at 73° C. and then cooling to 13° C., a 10 N aqueous solution of sodium hydroxide (60 cc) and then 1-bromo-4-chlorobutane (85 g) are added, whilst stirring, and stirring is continued for 15 hours at a temperature of about 20° C. The reaction mixture is then extracted three times with methylene chloride (430 cc in total); the organic extracts are combined, washed with distilled water (300 cc); dried over anhydrous sodium sulphate and filtered. The solution is poured onto neutral silica gel (100 g) contained in a column of diameter 3 cm; the column is eluted with methylene chloride (3700 cc). The first fraction (700 cc) is discarded. The second (2000 cc) is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at 35° C. Pyrid-2-ylmethyl 4-chlorobutyl sulphide (82 g) is thus obtained.

1. customthe temperature below 15° C.
2. temperaturecooling to 13° C.
3. stirringstirring
4. extractionThe reaction mixture is then extracted three times with methylene chloride (430 cc in total)
5. washwashed with distilled water (300 cc)
6. dry with materialdried over anhydrous sodium sulphate
7. filtrationfiltered
8. additionThe solution is poured onto neutral silica gel (100 g)
9. washthe column is eluted with methylene chloride (3700 cc)
10. concentrationThe second (2000 cc) is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at 35° C