反应详情

温度

78 °C

To a solution of 3,4-diaminotoluene (20.0 g, 162.6 mmol) and potassium hydroxide (11.36 g, 203.0 mmol) in H2O (40 mL) and MeOH (150 mL) was added carbon disulfide (13.3 mL, 220.8 mmol) slowly via syringe, and the reaction was heated to 78° C. for 2.5 hours. The mixture was poured over a mixture of ice (200 mL) and acetic acid (30 mL), and thick yellow precipitate formed. The mixture was stirred at 45° C. for 30 minutes, and then filtered to collect the solid precipitate, which was washed twice with H2O (40 mL total). The filter cake was triturated in a minimum of EtOAc, and then filtered and dried to give the title compound.

1. customformed
2. filtrationfiltered
3. customto collect the solid precipitate, which
4. washwas washed twice with H2O (40 mL total)
5. customThe filter cake was triturated in a minimum of EtOAc
6. filtrationfiltered
7. customdried