反应 #1075054
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07205302B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Under an argon atmosphere, a solution of 10.40 g of N-methoxy-N-methyl-p-toluamide in 100 ml of tetrahydrofuran was ice-cooled and 4-methylbenzylmagnesium chloride (solution prepared by dissolving 10.60 g of α-chloro-p-xylene and 1.94 g of magnesium in 85 ml of tetrahydrofuran) was added dropwise. After stirring for one hour, 100 ml of 10% hydrochloric acid was slowly added. The reaction solution was diluted with water, extracted with diethyl ether, washed with water and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the crude crystal was washed with diisopropyl ether and then dried under reduced pressure to obtain 8.43 g of the desired compound as a colorless crystal having a melting point of 93 to 100° C. cooled extracted with diethyl ether washed with water dried over anhydrous magnesium sulfate The solvent was evaporated under reduced pressure the crude crystal was washed with diisopropyl ether dried under reduced pressure
来源 ID: ord-da645eb9e0324749b0b8bb79768544e9