反应详情

温度

40 °C

To a solution of 4-anisidine (6.5 mmol, 800 mg) and DIEA (7.2 mmol, 1.24 mL) in CH2Cl2 (10 mL) cooled to 0° C. was added thiophosgene (6.5 mmol, 500 μL) dropwise. The solution was allowed to reach ambient temperature for 1 h, and 4,5-dichloro-1,2-phenylenediamine (6.5 mmol, 1.15 g) was added to the reaction. The reaction mixture was heated at 40° C. for 16 h, and MeI (7.2 mmol, 445 μL) and DIEA (7.2 mmol, 1.24 μL) were added. The reaction was heated at 40° C. for 8 h, and allowed to stand at ambient temperature for 16 h. Aqueous workup with CH2Cl2/brine, followed by flash chromatography on silica eluting with 4% MeOH in CH2Cl2 afforded the product as a brown oil. LC-MS (ESI, Method B): 1.62 min, m/z 308.2 (M+1).

1. temperatureThe reaction was heated at 40° C. for 8 h
2. waitto stand at ambient temperature for 16 h