反应详情

To dimethylformamide was added 92 mg of 1-chloro-5-phenylpentane and 152 mg of potassium iodide under ice-cooling, the mixture was allowed to warm up to room temperature and stirred for 20 minutes. Then, 200 mg of 5-(3,5-dichlorophenylthio)-4-isopropyl-2-(p-methoxybenzyloxymethyl)-1H-imidazole (101b)was added, followed by addition of 126 mg of potassium carbonate. Then the mixture was warmed up to 50° C. and allowed to react for 6 hours. After completion of the reaction, the mixture was diluted with water, extracted with diethyl ether, the extract was dried over sodium sulfate, and the solvent was distilled off under reduced pressure. To thus-obtained oil were added 10 ml of ethanol and 20 ml of 36% hydrochloric acid, and the mixture was stirred at 90° C. for 2 hours. After completion of the reaction, the solvent was distilled off under reduced pressure, an aqueous sodium hydrogen carbonate solution was added, extracted with ethyl acetate, the extract was dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (hexane:ethyl acetate=1:1)to give 120 mg of Compound I-124 (yield 57%).

1. temperaturecooling
2. temperatureThen the mixture was warmed up to 50° C.
3. customto react for 6 hours
4. customAfter completion of the reaction
5. extractionextracted with diethyl ether
6. dry with materialthe extract was dried over sodium sulfate
7. distillationthe solvent was distilled off under reduced pressure
8. customTo thus-obtained oil
9. stirringthe mixture was stirred at 90° C. for 2 hours
10. customAfter completion of the reaction
11. distillationthe solvent was distilled off under reduced pressure
12. additionan aqueous sodium hydrogen carbonate solution was added
13. extractionextracted with ethyl acetate
14. dry with materialthe extract was dried over sodium sulfate
15. distillationthe solvent was distilled off under reduced pressure
16. customThe residue was purified by silica gel chromatography (hexane