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欧阳幻实

新虫 (小有名气)

应助: 0 (幼儿园)
金币: 265.2
散金: 11
帖子: 76
在线: 15.7小时
虫号: 4555652
注册: 2016-03-30
性别: GG
专业: 有机合成

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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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注册: 2005-06-04
专业: 合成药物化学

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欧阳幻实(空位代发): 金币+30, 感谢应助 2016-08-10 20:46:04

于一个配有回流冷凝器的250毫升圆底烧瓶中,(Aldrich)溶于100毫升无水甲醇当中,向其中加入2滴三氟甲磺酸。加热回流48小时后用150毫升水骤冷再用200毫升戊烷分四份提取。水洗并用无水硫酸镁干燥之后,蒸出溶剂。通过吸附剂矾土过滤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。通过于一个配有回流冷凝器的100毫升圆底烧瓶中，将0.1摩尔的不对称N,N -二甲基阱加到0.05摩尔的羰基化合物中制备N,N -二甲腙。加热回流约12小时后，旋转蒸发除去过量的N,N二甲基阱。蒸馏油状物得到产物N,N -二甲腙。对甲苯磺酰腙。通过常规方式制备对甲苯磺酰腙。41羧酸肼类化合物。以常规方式方式通过酯类与水合肼反应制备羧酸肼类化合物。41N,N -二甲基烷基胺类。通过Icke, Wisegarver和A l l e ~的方法制备N,N -二甲基烷基胺类。~ *50毫升的80%甲酸于一个配有回流冷凝器的100毫升圆底烧瓶中，磁力搅拌下向其中缓慢加入0.05摩尔烷基胺随后加入8.1克的37%甲醛水溶液。反应物加热到80-90℃直至气体开始逸出为止。终止加热20分钟后再次加热回流8 - 12小时。将大约100毫升4N的HCI加入冷却了的溶液中,旋转蒸发溶液得到一种黄色油状物。通过加入50-75毫升的水随后加入50毫升的18 N NaOH溶液使游离胺释出。分离有机相，基本相用50毫升苯分两份提取。合并的有机相用水洗再用无水硫酸镁干燥。蒸出溶剂得到N,N -二甲胺,通过红外表征为不含伯胺，无需进一步提纯即可使用。N,N -二甲基金刚烷胺。通过B o r ~ h的方法制备N,N -二甲基金刚烷胺。~ ~于一个100毫升圆底烧瓶中，3.24克( 0.04摩尔)盐酸二甲胺溶于25毫升的甲醇中，向其中加入1.5克氢氧化钾片。一旦KOH溶解就将4.5克( 0.03摩尔)的2 -金刚烷酮加入并搅拌溶液15分钟。然后将氰基硼氢钠(0.63克, 0.01摩尔)加到10毫升甲醇中。 30分钟后将约2.0克的KOH溶于反应混合物中。通过旋转蒸发浓缩反应混合物,加入10毫升氯化钠水溶液之后分离有机相。水相用30毫升二乙醚分两份提取。合并的水相用50毫升6 M的HCI提取。酸提取物用二乙醚洗涤然后冷却到0℃并用KOH碱化。基本相用75毫升二乙醚分两份提取,合并提取物并用水和氯化钠水溶液洗,得到2.20克(41%收率)的N,N -二甲基金刚烷胺: IR (纯样品) 2780和2830 (m,-CH3)cm-l。
肟类。
肟类的制备以常规方式方式通过盐酸羟胺与醛或酮的碱性溶液反应进行。过滤出结晶的衍生物,用冷的甲醇洗涤，无需进一步提纯即可进行反应。

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