반응 #59875

반응 방정식

(2,2-bis(fluoromethyl)-1,3-dioxan-5-yl)methanol

sodium hydride

4-chloro-2,3-dimethylpyridine 1-oxide

→

title compound

수율 60.6%

4-((2,2-bis(fluoromethyl)-1,3-dioxan-5-yl)methoxy)-2,3-dimethylpyridine 1-oxide

수율 60.6%

용매

dimethylsulfoxide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added at room temperature
2. 2
   온도After the reaction mixture was cooled to room temperature
3. 3
   농축it was concentrated under reduced pressure
4. 4
   기타The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/methanol)

실험 절차

To a dimethylsulfoxide (10 ml) solution of the (2,2-bis(fluoromethyl)-1,3-dioxan-5-yl)methanol (1.6 g, 8.98 mmol) obtained in the step (7a), sodium hydride, in oil (431 mg, 9.88 mmol as the content was regarded as 55%) was added at room temperature. To the mixture, 4-chloro-2,3-dimethylpyridine 1-oxide (1.42 g, 8.98 mmol) was added and the mixture was stirred at 60° C. for 2 hours. After the reaction mixture was cooled to room temperature, it was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/methanol) to obtain the title compound (1.63 g, yield: 60.6%) as a yellow oil.

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