反应详情

温度

60 °C

A mixture of the compound (0.1 g) obtained in Example 4, dimethylcarbamothioyl chloride (25 mg), triethylamine (76 mg) and N,N-dimethylformamide (2 ml) was stirred at 60° C. for 3 hr. The reaction mixture was diluted with ethyl acetate, 5% aqueous potassium hydrogen sulfate solution, washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over anhydrous sodium sulfate, and is concentrated under reduced pressure. The residue was purified by column chromatography [developing solvent:ethyl acetate-hexane (3:1, volume ratio)], and recrystallized from ethyl acetate-hexane (1:1, volume ratio) to give the title compound (40 mg) as a colorless powder.

1. washwashed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
2. dry with materialdried over anhydrous sodium sulfate
3. concentrationis concentrated under reduced pressure
4. customThe residue was purified by column chromatography [developing solvent:ethyl acetate-hexane (3:1, volume ratio)]
5. customrecrystallized from ethyl acetate-hexane (1:1, volume ratio)