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欧阳幻实新虫 (小有名气)
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(Aldrich) dissolved in 100 mL of absolute methanol in a 250-mL round-bottom flask equipped with reflux condenser was added 2 drops of trifluoromethanesulfonic acid. After heating under reflux for 48 h, the reaction was quenched with 150mL of water and extracted with 200 mL of pentane in four portions. After washing with water and drying over anhydrous magnesium sulfate, the solvent was evaporated. Filtration of the crude oil dissolved in benzene through adsorbent alumina yielded 4.9 g (74% yield) of benzhydryl methyl ether. N,N-Dimethylhydrazones. N,N-Dimethylhydrazones were prepared by adding 0.1 mol of unsymmetrical N,N-dimethylhydrazine to 0.05 mol of carbonyl compound in a 100-mL round-bottom flask equipped with reflux condenser. After heating under reflux for ca. 12 h, the excess N,N-dimethylhydrazine was removed by rotary evaporation. The product oil was distilled to yield the product N,N-dimethylhydrazone. p-Toluenesulfonylhydrazones.p-Toluenesulfonylhydrazones were prepared in the usual manner.41 Carboxylic Acid Hydrazides. Carboxylic acid hydrazides were prepared in the usual manner by reaction of the ester with hydrazine hydrate.41 N,N-Dimethylalkylamines.N,N-Dimethylalkylamines were prepared by the method of Icke, Wisegarver, and A l l e ~ . ~ *To 50 mL of 80% formic acid in a magnetically stirred 100-mL round-bottom flask equipped with a reflux condenser was slowly added 0.05 mol of alkyl amine followed by 8.1 g of 37% aqueous formaldehyde.The reaction was heated to 80-90 OC until gas evolution commenced. After 20 min without heating, the flask was again heated under reflux for 8-12 h. To the cooled solution was added ca. 100 mL of 4 N HCI, and the solution was rotary evaporated to yield a yellow oil. The free amine was liberated by the addition of 50-75 mL of water followed by 50 mL of 18 N NaOH solution. The organic phase was separated and the basic phase was extracted with 50 mL of benzene in two portions. Thecombined organic phases were washed with water and dried over anhydrous magnesium sulfate. Evaporation of the solvent yielded the N,N-dimethylamine, characterized by IR as being free of primary amine, which was used without further purification. N,N-Dimethyladamantylamine.N,N-Dimethyladamantylamine was prepared by the method of B o r ~ h . ~ ~To 3.24 g (0.04 mol) of dimethylamine hydrochloride dissolved in 25 mL of methanol in a 100-mLround-bottom flask was added 1.5 g of potassium hydroxide pellets. Upon dissolution of the KOH, 4.5 g (0.03 mol) of 2-adamantanone was added and the solution was stirredfor 15 min. Sodium cyanoborohydride(0.63 g, 0.01 mol) was then added to 10 mL of methanol. After 30 min, ca. 2.0 g of KOH was dissolved in the reaction mixture. The reaction mixture was concentrated by rotary evaporation, and followingthe addition of 10 mL of aqueous sodium chloride the organic phase was separated. The aqueous phase was extracted with 30 mL of diethyl ether in two portions. The combined aqueous phases were extracted with 50 mL of 6 M HCI. The acid extracts were washed with diethyl ether and then cooled to 0 OC and basified with KOH. Extraction of the basic phase with 75 mL of diethyl ether in two portions, which were combined and washed with water and aqueous sodium chloride, yielded 2.20 g (41% yield) of N,N-dimethyladamantylamine: IR (neat) 2780 and 2830 (m, -CH3) cm-l. Oximes. Oximes were prepared in the usual manner by reaction of hydroxylamine hydrochloride with a basic solution of the aldehyde or ketone. The crystalline derivatives were filtered, washed with cold methanol, and reacted without further purification. |
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