反应详情

Into a 500 ml reactor were charged o-toluidine (27 g), sulfur (8g), and carbon disulfide (22 g). Seventy minutes of electrically heating the system was required to elevate the temperature to 275°C (240 psig original pressure at 275°C). After 21/2 hours at 275°C (the pressure leveled out at 470 psig in 90 minutes) the heat source was removed and the reactor was cooled. The reaction mixture was mixed with 200 g water containing 16 g sodium hydroxide. Tar-like residue (18.5 g) was removed by decantation. Acidification of decantate with hydrochloric acid and filtration of the resulting mixture gave 21 g (46 percent yield) of crude 2-mercapto-4-methylbenzothiazole (m.p. 161°-173°C).

1. temperatureSeventy minutes of electrically heating the system
2. customto 275°C
3. custom(240 psig original pressure at 275°C)
4. custom) the heat source was removed
5. temperaturethe reactor was cooled
6. additionThe reaction mixture was mixed with 200 g water containing 16 g sodium hydroxide
7. customTar-like residue (18.5 g) was removed by decantation
8. filtrationAcidification of decantate with hydrochloric acid and filtration of the resulting mixture