反应 #533181

反应方程式

diisobutylaluminum hydride toluene

hydrochloric acid

4,4-difluoro-N-methoxy-N-methylcyclohexane-1-carboxamide

4,4-Difluoro-N-methoxy-N-methylcyclohexane-1-carboxamide

diisobutylaluminum hydride toluene

→

title compound

收率 115.1%

4,4-Difluorocyclohexane-1-carbaldehyde

收率 115.1%

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   workup.STIRRINGthe reaction mixture was stirred at −70° C. for two hours
2. 2
   萃取was extracted with ethyl acetate
3. 3
   干燥The organic layer was dried over magnesium sulfate
4. 4
   workup.DISTILLATIONthe solvent was distilled off

实验过程

A mixture of 4,4-difluoro-N-methoxy-N-methylcyclohexane-1-carboxamide obtained in Example 2a (1.7 g, 8.21 mmol) and tetrahydrofuran (60 ml) was cooled to −70° C., a 1.0 M diisobutylaluminum hydride/toluene solution (9.85 ml, 9.85 mmol) was added, and the reaction mixture was stirred at −60° C. for 35 minutes. A 1.0 M diisobutylaluminum hydride/toluene solution (5 ml, 5 mmol) was further added at −65° C., and the reaction mixture was stirred at −70° C. for two hours. A 2 N aqueous hydrochloric acid solution was added to the reaction mixture, which was extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, and the solvent was distilled off to give a crude product of the title compound (1.4 g).

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