反应详情

A mixture of 3-[N-(2,6-dimethylphenyl)carbamoyl]-4-methoxy-5-chloroaniline (650 mg), diethylthiocarbamoyl chloride (360 mg) and chlorobenzene (6 ml) is refluxed for 30 minutes. The reaction mixture is mixed with water and shaken with methylene chloride. The organic layer is washed with water, dried over Glauber's salt and concentrated to remove the solvent. The residue is chromatographed on a column of silica gel, which is eluted with methylene chloride. The eluted fractions are collected and the solvent is evaporated. The residue is recrystallized from ethyl acetate to give 3-[N-(2,6-dimethylphenyl)carbamoyl]-4-methoxy-5-chlorophenyl isothiocyanate (340 mg) as crystals melting at 191°-192.5° C.

1. temperatureis refluxed for 30 minutes
2. washThe organic layer is washed with water
3. dry with materialdried over Glauber's salt
4. concentrationconcentrated
5. customto remove the solvent
6. customThe residue is chromatographed on a column of silica gel, which
7. washis eluted with methylene chloride
8. customThe eluted fractions are collected
9. customthe solvent is evaporated
10. customThe residue is recrystallized from ethyl acetate