In a 500ml wide-mouthed Erlenmeyer

In a 500ml wide-mouthed Erlenmeyer flask, aluminum foil (10g, 0.37 mol) cut to 3x3cm pieces was amalgamated in a solution of 200 mg HgCl2 in 400 ml warm water until the solution became greyish, and hydrogen bubbles was evolved in a steady rate from the aluminum surface. The water was decanted, and the amalgamated aluminum pieces were washed twice with 250ml cold water.
To the aluminum amalgam (still in the above flask) there was added, quickly, a 40% Methylamine solution (43 mL, 0.50 mol), isopropanol (100 mL), Phenyl-2-Propanone (13.42g, 0.10 mol), and finally another 100 mL isopropanol (which was used to rinse the beaker the P2P had been in). The aluminum pieces were poked with a glass rod so that all of them were below the surface of the liquid. Hydrogen began to evolve vigorously from the aluminum surface, and the temperature (which was measured by a small thermometer inserted into the flask) rose quickly. The evaporation of methylamine was attenuated by covering the mouth of the flask with some Al foil (do not plug it tight, or it may explode), and the reaction rate was controlled by immersing the reaction flask in cold water from time to time during the first hour so that the temperature did not rise over 50°C. At the 2 hour point most of the aluminum was consumed, and 20 mL 25% aqueous NaOH was added to the solution and magnetic stirring was initiated (keep an eye on the temperature again, and keep it below 50°C). At the 3 hour point another 20 mL 25% NaOH was added (no significant temp rise), whereafter it was allowed to stir at room temp overnight and then allowed to settle.
The clear supernatant was decanted, 100ml isopropanol was added to the grey sludge, it was stirred for another hour, and the supernatant again decanted after the particle suspension had settled. The aluminum sludge at the bottom of the flask was now vacuum filtered through an inch of Celite in a buchner funnel and washed with 2 x 50 mL methanol. All the decantations and washes were combined, and the solution concentrated under vacuum.
The residue was taken up in 300 mL water, acidified with conc. HCl, washed with 3x50ml methylene chloride, basified with 25% NaOH, and extracted with 3x100ml ethyl acetate. The combined organic extracts were washed with 75ml brine, followed by drying over anhydrous sodium sulfate with good magnetic stirring for 15 min. The drying agent was removed by filtration from the crystal-clear solution and the solvent distilled off on an oil-bath heated to no more than 110°C (as to not risk any evaporation of the freebase). The residue was taken up in 150 mL diethyl ether and with good stirring a solution of 5M HCl in isopropanol was added until the solution was acid to dampened universal pH paper. The precipitate was filtered off with suction using a fritted glass funnel and the filter cake was washed with 2 x 50 mL ether and sucked dry. After air-drying overnight on a plate, the crude product (13.6 g) still had a strong solvent smell, and was recrystallized by dissolving it in 65 mL acetonitrile (5 mL/gram), and quickly vacuum filtering the hot solution through a fritted glass funnel to remove a slight turbidity, and the solution was then left at room temp to crystallize, and after about an hour the white crystalline precipitate was filtered with suction, washed with 2 x 25 mL ether and air dried. The filtrate and ether washes (collected separately) were both cooled to -20°C in the freezer, and from the acetonitrile a second crop was collected, while nothing came out of the ether.

結果 (中文) 1:

在 500 毫升宽口锥形瓶，铝箔 （10g、 0.37 mol） 切 3x3cm 碎被合并 400 毫升温水 200 毫克 HgCl2 溶液中直到解决方案变得灰白，和氢气泡在以稳定的速率从铝表面演变而来。合并后的铝片冲了两次用 250 毫升冷水与水倒出。（仍在上述瓶） 铝汞又增加了，很快，40%甲胺溶液 （43 毫升，0.50 mol）、 异丙醇 （100 毫升）、 苯基-2-丙酮 （13.42 g，0.10 mol），最后另一 100 mL 异丙醇 （这用来冲洗 P2P 已经在烧杯）。所以，他们都是液体的表面之下铝片被用一根玻璃棒捅了捅。氢开始从铝表面，大力发展和温度 （这衡量小温度计插入瓶） 迅速攀升。甲胺蒸发减弱所覆盖的带一些铝箔 （做不插它紧，或它可能会爆炸），瓶嘴和反应速率受浸烧瓶在冷水中的第一个小时内，温度没有上升超过 50 ° c。在 2 个小时点铝大部分被消耗，并发起了 20 毫升 25%氢氧化钠水溶液被添加到解决方案和电磁搅拌 （再次，保持眼睛对温度和保持低于 50 ° C）。在 3 小时点另一个 20 毫升 25%氢氧化钠被添加 （没有重大的温度上升），随后它被允许在室温搅拌一夜之间，然后获准定居。倒出清，100 毫升异丙醇被添加到灰色的污泥，它打动了另一个小时，和上清液再一次倒出后粒子悬浮剂已经解决了。铝型材厂污泥在瓶底现在是真空过滤通过硅藻土在布氏漏斗英寸和 2 x 50 毫升甲醇用清水洗净。所有的了解和洗相结合，和解决方案集中在真空状态下。残留物被占去了 300 毫升水中，用混凝土盐酸酸化，3x50ml 二氯甲烷用清水洗净，碱化与 25%氢氧化钠，和 3x100ml 乙酸乙酯提取物。复合有机提取物被冲走 75 毫升盐水后，紧接着在用好电磁搅拌 15 分钟无水硫酸钠干燥。从清澈见底的解决方案和溶剂蒸馏出油浴加热到不超过 110 ° C （对于不冒任何的化学蒸发） 过滤除去乾燥剂。残留物被 150 毫升乙醚和好搅拌 5 M HCl 中异丙醇溶液添加，直到解决的办法是向被挫伤普遍 pH 试纸酸。沉淀过滤掉吸用熔块的玻璃漏斗，2 x 50 毫升醚用清水洗净并吸干了滤饼。后风干一夜之间在一个盘子上，粗品 (13.6 g) 仍有较强的溶剂气味，通过溶解在乙腈 65 毫升 （5 毫升/克），进行重结晶和快速真空过滤通过烧结的玻璃漏斗，以去除轻微的浊度，热解决方案解决方案是然后室温结晶，和离开后大约一小时白色结晶沉淀过滤吸2 × 25 毫升醚和空气干燥用清水洗净。（分别收集） 的滤液和醚洗了两个冷却到-20 ° C 在冰箱里，和从乙腈二作物收集了，虽然没有产生任何醚。

結果 (中文) 3:

在500ml广口瓶、铝箔（10g，0.37 mol）切3x3cm碎片合并在一个200毫克的HgCl2溶液在400毫升温水直到溶液变成灰，和氢气泡是进化稳定的速度从铝表面。水倒出，和合并的铝片250ml冷水洗两次。对铝汞齐（仍在上述瓶）有加，很快，40%甲胺水溶液（43 mL，0.50 mol），异丙醇（100毫升），phenyl-2-propanone（13.42g，0.10 mol），最后一个100 ml异丙醇（这是用来冲洗烧杯P2P已经在）。铝片用玻璃棒都低于表面的液体。氢开始从铝表面大力发展，并用一个小温度计插入瓶内测量的温度迅速上升。甲胺的蒸发是通过覆盖一些铝箔烧瓶口衰减（不插紧它，或者它可能会爆炸），和反应速率是通过将反应瓶冷水从时间到时间的一个小时内使温度上升不超过50°在2小时点大部分的铝消耗的控制，和20毫升25%水NaOH被添加到解决方案和磁力搅拌开始（注意，温度保持50°C以下）。在3小时的时候另一个20毫升加入25% NaOH（无明显温升），然后它可以搅拌室温过夜然后可以沉淀。上清液倒出，100ml异丙醇添加到灰色的污泥，这是搅拌一小时，然后再倒出上清液后悬浮颗粒定居。在烧瓶底部的铝污泥真空过滤现在在毕希纳漏斗一寸- 2 x 50 mL甲醇洗。所有移注和洗相结合，与溶液经真空浓缩。残余物在水300毫升，加浓。盐酸，与3x50ml二氯甲烷洗涤，用25%的NaOH，和3x100ml乙酸乙酯提取。合并有机提取物有75ML的盐水洗涤，然后干燥和良好的磁搅拌15 min干燥剂无水硫酸钠通过过滤除去从清澈的溶液和溶剂蒸馏脱油浴加热到不超过110°C（以不冒任何蒸发的Freebase）。残留了150毫升乙醚和良好的搅拌5M HCl溶液中异丙醇添加到溶液呈酸性的pH试纸蘸通用。将沉淀过滤掉用烧结玻璃漏斗和滤饼吸用2 x 50毫升乙醚洗涤，吸干。空气干燥过夜，在板后，原油产品（13.6克）仍具有较强的溶剂气味，被溶解在65 mL乙腈结晶（5毫升/克），和快速真空过滤热溶液通过烧结玻璃漏斗将轻微浑浊，并将溶液在室温临时离开结晶，经过大约一个小时的白色结晶沉淀过滤抽吸，2 x 25毫升乙醚和空气洗干。滤液和醚洗（分别收集）被冷却到20°C在冰箱里，从乙腈第二个作物被收集，而没有出来的醚。