反应详情

With cooling with ice, sodium borohydride (5.5 g, 134 mmol) was added to a dichloromethane (500 mL)/methanol (500 mL) mixed solution of 2-[(2-hydroxyphenyl)thio]-1-{4-[(triisopropylsilyl)oxy]phenyl}propan-1-one (48 g, 112 mmol) obtained in Reference Example 1-2, and stirred for 2 hours with cooling with ice, then restored to room temperature, and further stirred for 40 minutes. Aqueous saturated ammonium chloride solution was added, and stirred for a while, and then the solvent was almost completely evaporated off under reduced pressure. The residue was diluted with ethyl acetate, and extracted with aqueous saturated ammonium chloride solution. The organic layer was dried with sodium sulfate, and concentrated under reduced pressure to obtain a crude product (51.4 g) of the intended compound.

1. customobtained in Reference Example 1-2
2. temperaturewith cooling with ice
3. customrestored to room temperature
4. stirringfurther stirred for 40 minutes
5. stirringstirred for a while
6. customthe solvent was almost completely evaporated off under reduced pressure
7. additionThe residue was diluted with ethyl acetate
8. extractionextracted with aqueous saturated ammonium chloride solution
9. dry with materialThe organic layer was dried with sodium sulfate
10. concentrationconcentrated under reduced pressure