反应详情

In dichloromethane (10 ml) was dispersed 1-[(2R,3R)-3-(2,4-difluorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)-2-butylsulfonyl]piperazine.dihydrochloride (Compound 20, 0.20 g) obtained in Working Example 14. To the dispersion were added, under ice-cooling, triethylamine (0.20 ml) and 4-trifluoromethylbenzoyl chloride (0.13 g). The mixture was stirred for 30 minutes at room temperatures. The reaction mixture was then concentrated under reduced pressure. The concentrate was dissolved in ethyl acetate, washed with water, dried and concentrated. The concentrate was subjected to a silica gel chromatography (eluent: hexane/ethyl acetate=1/3) for purification. The object fraction was concentrated which was processed with hydrogen chloride, followed by adding thereto isopropylether to give 1-[(2R,3R)-3-(2,4-difluorophenyl)-3-hydroxy-4-(1H-1,2,4-triazol-1-yl)-2-butylsulfonyl]-4-(4-trifluoromethylbenzoyl)piperazine (Compound 24).hydrochloride (167 mg) as colorless powder.

1. customobtained in Working Example 14
2. additionTo the dispersion were added, under ice-
3. temperaturecooling
4. concentrationThe reaction mixture was then concentrated under reduced pressure
5. dissolutionThe concentrate was dissolved in ethyl acetate
6. washwashed with water
7. customdried
8. concentrationconcentrated
9. customThe concentrate was subjected to a silica gel chromatography (eluent: hexane/ethyl acetate=1/3) for purification
10. concentrationThe object fraction was concentrated which
11. additionby adding