反应详情

温度

2.5 °C

To a solution of (2R)-2-[4-{[3,5-bis(trifluoromethyl)phenyl]acetyl}-2-(3,4-dichlorophenyl)morpholin-2-yl]ethanol obtained in Reference Example 1 (3.0 g, 5.7 mmol) in methylene chloride (30 ml) were added dimethylaminopyridine (0.07 g, 0.57 mmol) and triethylamine (1.2 ml, 8.5 mmol) under a nitrogen stream, the resulting mixture was cooled to 0-5° C., and then a solution of 4-methylbenzenesulfonyl chloride (1.3 g, 6.8 mmol) in methylene chloride (10 ml) was further added dropwise at below 10° C. with stirring. After the resulting mixture was stirred at room temperature for 8 hours, to the reaction mixture were added water (30 ml) and concentrated hydrochloric acid (1 ml), and the resulting mixture was partitioned. The separated organic layer was washed with water (30 ml) and evaporated to dryness. The residue obtained was purified by chromatography on a silica gel column and then crystallized from a mixed solvent of toluene (7 ml) and methylcyclohexane (35 ml) under ice-cooling to afford the title compound [2.3 g, yield: 60.3%] as a colorless crystalline solid.

1. stirringAfter the resulting mixture was stirred at room temperature for 8 hours, to the reaction mixture
2. customthe resulting mixture was partitioned
3. washThe separated organic layer was washed with water (30 ml)
4. customevaporated to dryness
5. customThe residue obtained
6. customwas purified by chromatography on a silica gel column
7. customcrystallized from a mixed solvent of toluene (7 ml) and methylcyclohexane (35 ml) under ice-
8. temperaturecooling