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歐陽幻實(shí)

新蟲 (小有名氣)

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金幣: 265.2
散金: 11
帖子: 76
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蟲號: 4555652
注冊: 2016-03-30
性別: GG
專業(yè): 有機(jī)合成

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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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歐陽幻實(shí)(空位代發(fā)): 金幣+30, 感謝應(yīng)助 2016-08-10 20:46:04

于一個(gè)配有回流冷凝器的250毫升圓底燒瓶中,(Aldrich)溶于100毫升無水甲醇當(dāng)中,向其中加入2滴三氟甲磺酸。加熱回流48小時(shí)后用150毫升水驟冷再用200毫升戊烷分四份提取。水洗并用無水硫酸鎂干燥之后,蒸出溶劑。通過吸附劑礬土過濾溶于苯中的粗油得到4.9克( 74%收率)二苯甲基甲醚。
N,N -二甲腙。通過于一個(gè)配有回流冷凝器的100毫升圓底燒瓶中，將0.1摩爾的不對稱N,N -二甲基阱加到0.05摩爾的羰基化合物中制備N,N -二甲腙。加熱回流約12小時(shí)后，旋轉(zhuǎn)蒸發(fā)除去過量的N,N二甲基阱。蒸餾油狀物得到產(chǎn)物N,N -二甲腙。對甲苯磺酰腙。通過常規(guī)方式制備對甲苯磺酰腙。41羧酸肼類化合物。以常規(guī)方式方式通過酯類與水合肼反應(yīng)制備羧酸肼類化合物。41N,N -二甲基烷基胺類。通過Icke, Wisegarver和A l l e ~的方法制備N,N -二甲基烷基胺類。~ *50毫升的80%甲酸于一個(gè)配有回流冷凝器的100毫升圓底燒瓶中，磁力攪拌下向其中緩慢加入0.05摩爾烷基胺隨后加入8.1克的37%甲醛水溶液。反應(yīng)物加熱到80-90℃直至氣體開始逸出為止。終止加熱20分鐘后再次加熱回流8 - 12小時(shí)。將大約100毫升4N的HCI加入冷卻了的溶液中,旋轉(zhuǎn)蒸發(fā)溶液得到一種黃色油狀物。通過加入50-75毫升的水隨后加入50毫升的18 N NaOH溶液使游離胺釋出。分離有機(jī)相，基本相用50毫升苯分兩份提取。合并的有機(jī)相用水洗再用無水硫酸鎂干燥。蒸出溶劑得到N,N -二甲胺,通過紅外表征為不含伯胺，無需進(jìn)一步提純即可使用。N,N -二甲基金剛烷胺。通過B o r ~ h的方法制備N,N -二甲基金剛烷胺。~ ~于一個(gè)100毫升圓底燒瓶中，3.24克( 0.04摩爾)鹽酸二甲胺溶于25毫升的甲醇中，向其中加入1.5克氫氧化鉀片。一旦KOH溶解就將4.5克( 0.03摩爾)的2 -金剛烷酮加入并攪拌溶液15分鐘。然后將氰基硼氫鈉(0.63克, 0.01摩爾)加到10毫升甲醇中。 30分鐘后將約2.0克的KOH溶于反應(yīng)混合物中。通過旋轉(zhuǎn)蒸發(fā)濃縮反應(yīng)混合物,加入10毫升氯化鈉水溶液之后分離有機(jī)相。水相用30毫升二乙醚分兩份提取。合并的水相用50毫升6 M的HCI提取。酸提取物用二乙醚洗滌然后冷卻到0℃并用KOH堿化。基本相用75毫升二乙醚分兩份提取,合并提取物并用水和氯化鈉水溶液洗,得到2.20克(41%收率)的N,N -二甲基金剛烷胺: IR (純樣品) 2780和2830 (m,-CH3)cm-l。
肟類。
肟類的制備以常規(guī)方式方式通過鹽酸羥胺與醛或酮的堿性溶液反應(yīng)進(jìn)行。過濾出結(jié)晶的衍生物,用冷的甲醇洗滌，無需進(jìn)一步提純即可進(jìn)行反應(yīng)。

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