反应详情

Then, 0.40 g (0.88 mM) of 2-oxooctyl-(6-decyloxy-2-naphthoyl)amine, 0.38 g (0.94 mM) of Lawesson's reagent and 6 ml of tetrahydrofuran were placed in a 30 ml-round-bottomed flask, followed by heat-refluxing for 45 minutes under stirring. After the reaction, the reaction mixture was poured into a solution of 0.27 g of sodium hydroxide in 70 ml of ice water to precipitate a crystal. The crystal was recovered by filtration washed with water and dissolved in toluene, followed by drying with anhydrous sodium sulfate and distilling-off of the solvent under reduced pressure. The residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/1) and recrystallized from a mixture solvent of acetonemethanol to obtain 0.21 g of 2-(6-decyloxy-2-naphthyl)-5-hexylthiazole (Yield: 52.7%). ##STR236##

1. temperatureby heat-refluxing for 45 minutes
2. customAfter the reaction
3. customto precipitate a crystal
4. filtrationThe crystal was recovered by filtration
5. washwashed with water
6. dissolutiondissolved in toluene
7. dry with materialby drying with anhydrous sodium sulfate and distilling-off of the solvent under reduced pressure
8. customThe residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/1)
9. customrecrystallized from a mixture solvent of acetonemethanol