反应详情

1.00 g (2.59 mmol) of (rac.) 4-(4-chloro-3-fluoro-2-methoxyphenyl)-4-methyl-2-(trifluoromethyl)-2-hydroxy-pentanoic acid ethyl ester is dissolved in 9.5 ml of diethyl ether and mixed in portions at 0° C. with 73.7 mg (1.94 mmol) of LiAlH4. Stirring is continued at 0° C., and a TLC is taken every quarter hour. After 40 minutes of stirring at 0° C., the reaction mixture is mixed drop by drop with 2.4 ml of saturated NaHCO3 solution while being cooled in an ice bath. It is stirred for 30 minutes while being cooled in an ice bath, and it is stirred vigorously overnight at room temperature. The precipitate is suctioned off, washed with ethyl acetate, and the filtrate is concentrated by evaporation in a rotary evaporator. After the residue is chromatographed on a Flashmaster, 560.2 mg is obtained. In this case, this is a 3:2 mixture of the aldehyde with the starting ester.

1. customis continued at 0° C.
2. waita TLC is taken every quarter hour
3. stirringAfter 40 minutes of stirring at 0° C.
4. temperaturewhile being cooled in an ice bath
5. stirringIt is stirred for 30 minutes
6. temperaturewhile being cooled in an ice bath
7. stirringit is stirred vigorously overnight at room temperature
8. washwashed with ethyl acetate
9. concentrationthe filtrate is concentrated by evaporation in a rotary evaporator
10. customAfter the residue is chromatographed on a Flashmaster
11. custom560.2 mg is obtained