反应详情

2-{4-[(3,7-Dimethyl-2,6-octadienyl)oxy]phenyl}acetic acid (1.00 g,3.47 mmol) was dissolved in tetrahydrofuran (12 ml), and 1,1′-carbonyldiimidazole (0.68 g, 4.16 mmol) was added thereto. The mixture was stirred for 1 hour at room temperature, and then 3-amino-1,2,4-dithiazole-5-thione (0.42 g, 2.70 mmol) was added thereto. After being stirred for 3 hours at room temperature, the mixture, with water added thereto, was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over MgSO4, and then concentrated. The obtained residue was purified by silica gel chromatography (chloroform), to give 2-{4-[(3,7-dimethyl-2,6-octadienyl)oxy]phenyl}-N-(3thioxo-3H-1,2,4-dithiazol-5-yl)acetoamide (Compound 2) (0.187 g, 18%).

1. stirringAfter being stirred for 3 hours at room temperature
2. extractionwas extracted with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe obtained residue was purified by silica gel chromatography (chloroform)