4.4.2 Iron Reduction of 1-phenyl-2-

4.4.2 Iron Reduction of 1-phenyl-2-nitropropene to 1-phenyl-2-propanone

Pour 15 liters of clean tap water into the vessel. Follow this with 4000g of catalytic iron, 3400g (20mol) of 1-phenyl- 2-nitropropene and 40-50g of ferric chloride. Assemble the top with the condenser in the reflux mode, start the water running through the condenser, begin stirring, and fire up the propane burner. Watch the thermometer and turn off the heat when the temperature reaches 90癈. Slowly add muriatic acid in small doses over a 2-hour period. Watch the top of the condenser for signs things are getting out of hand. This reaction needs to be performed in a small shed or other outbuilding with good ventilation. Install a heavy-duty (500+cfm) exhaust fan in the shed. The reason for this is that the fumes from this reaction are very corrosive and if the reaction goes into runaway, one will want to abandon the shed for awhile as the fumes clear out. A total of 15 liters of muriatic acid is added. Once all of the acid has been added, allow the stirring to continue for another 2 hours before going on to the next step.

We now must extract our P2P from the nasty black mess inside the reaction vessel. We will do this through steam distillation. Disconnect the condenser, flange, and "Tee", leaving the 2" nipple open. The stirrer should remain turning. Next, quickly pour in about 4 liters of saturated lye solution that has cooled off overnight. Some heat and steam will be generated as the lye neutralizes the muriatic acid. Assemble the Tee, flange, and condenser in the distillation mode and start the water flowing through the condenser. Place a 20 liter bucket under the end and fire up the propane burner to high. Discontinue stirring. Distill over the water and P2P until the bucket is full, then turn off the heat.

The yield for this reduction is 75% no matter how badly one thinks he has blown it, so we should expect to obtain 15 moles, or a little over 2000g of P2P. Since P2P has a density close to that of water, this works out to about 2 liters of product.

We must now extract the P2P from the water, purify it, and store it for later use. This is accomplished by pouring 3000ml of water/P2P into each of two 4000ml separatory funnel. One then adds about 300ml of saturated lye solution to each and shakes vigorously for 3-5 minutes. This is done to insure there is no residual acid which can, and will, poison the catalyst when used. After a thorough shaking, 400ml of methylene chloride is added to each separatory funnel and shaken vigorously for 2-3 minutes. Methylene chloride is an easily obtainable solvent for most plastics. Check the plastics supply shops that sell buckets, sheet plastic, etc. Since methylene chloride is heavier than water, it will pick up the P2P and carry it to the bottom of the sep funnel. This takes some time, however, so one must not get in a hurry. This writer allows the separation to sit for 6 hours before draining the bottom layer into a one-gallon wine bottle, or even better, an amber glass bottle. Cut a square out of a plastic baggie and use it for a seal between the bottle-top and the cap. Add another 400ml of methylene chloride, shake vigorously, and let it settle out again for 6 hours before draining. This is good enough, go on to the next batch. When finished, one should have 3-4 gallons of methylene chloride/P2P solution.



We will now recover our methylene chloride solvent for reuse and distill the P2P. Use a 5000ml round-bottom vessel and distill over the methylene chloride from 39 to 60癈. Return the solvent to it's container and continue until there is only about 2000ml of P2P left in the vessel. Add boiling stones and vacuum distill over the remnants of the methylene chloride and water until it is clear that only P2P is left. Using a clean receiver and fresh boiling stones, distill over the P2P at 105-115癈. Do not distill at a temperature lower than 105癈 or the P2P will carry contaminants over with it, the contaminants being darker colored. P2P is a clear, pale-yellow liquid that smells like cat piss. P2P will auto- oxidize over a period of weeks if left at room temperature, so put it in the freezer until ready for use.

One can use toluene to extract the P2P from the water, but it must be vacuum-distilled and the separation will be to the top instead of the bottom like methylene chloride. It takes about the same amount of time to separate as when using methylene chloride.

結果 (中文) 1:

4.4.2 Iron Reduction of 1-phenyl-2-nitropropene to 1-phenyl-2-propanonePour 15 liters of clean tap water into the vessel. Follow this with 4000g of catalytic iron, 3400g (20mol) of 1-phenyl- 2-nitropropene and 40-50g of ferric chloride. Assemble the top with the condenser in the reflux mode, start the water running through the condenser, begin stirring, and fire up the propane burner. Watch the thermometer and turn off the heat when the temperature reaches 90癈. Slowly add muriatic acid in small doses over a 2-hour period. Watch the top of the condenser for signs things are getting out of hand. This reaction needs to be performed in a small shed or other outbuilding with good ventilation. Install a heavy-duty (500+cfm) exhaust fan in the shed. The reason for this is that the fumes from this reaction are very corrosive and if the reaction goes into runaway, one will want to abandon the shed for awhile as the fumes clear out. A total of 15 liters of muriatic acid is added. Once all of the acid has been added, allow the stirring to continue for another 2 hours before going on to the next step.我们现在必须从中提取我们 P2P 反应容器内的黑色一团糟。通过水蒸气蒸馏法，我们会这样做。断开连接的凝汽器、 法兰，和"三通"，使 2"乳头保持打开状态。搅拌器应继续转动。下一步，快速倒在 4 升左右的饱和的碱液解决方案，一夜之间已趋缓。因为碱液中和盐酸，将生成一些热量和蒸汽。组装三通、 法兰、 和凝汽器在蒸馏模式和开始通过冷凝器的流水。放在结束下的一 20 升桶和点燃丙烷燃烧器，高。停止搅拌。蒸馏的水和 P2P 直到桶充满，然后关火。这种减少的收益是无论多么一个认为他吹过它，所以我们应该期望得到 15 痣或稍微超过 2000 g 的 P2P 的 75%。由于 P2P 已接近水的密度，这相当于约 2 升的产品。我们现在必须从水中提取 P2P、 净化它，和存储供以后使用。这被通过浇注 3000 毫升的水/P2P 入每个两个 4000 毫升分液漏斗。一个将大约 300 毫升的饱和的碱液解决方案添加到每个然后摇大力为 3-5 分钟。这样做的目的是为了确保没有残留的酸，并将毒药催化剂时使用。彻底的握手后, 400 毫升的二氯甲烷是添加到每个分液漏斗，用力摇晃 2-3 分钟。二氯甲烷是一种很容易提炼出溶剂为大多数塑料。检查的塑料供应店卖桶、 塑料片等。由于二氯甲烷是比水重，它将拿起 P2P，叼到 sep 漏斗的底部。这需要一些时间，然而，这样一个不能急。这位作家允许分离坐 6 小时前底层水排入一加仑的葡萄酒瓶，或甚至更好，琥珀色的玻璃瓶。剪出一个塑料袋子的广场和使用它的瓶子的顶部和盖之间的密封。添加另一个 400 毫升的二氯甲烷、 摇大力，和让它沉淀下来了再 6 小时之前排水。这是不够好，转到下一批。完成后，一个人应该有 3 4 加仑的亚甲基氯/P2P 解决方案。 我们现在将重用我们亚甲基氯化溶剂回收和提炼 p2p 网络。使用 5000 毫升圆底容器，并在二氯甲烷从 39 到 60癈提炼。返回到它的容器的溶剂和继续，直到只有大约 2000 毫升的容器中的 P2P 左。添加沸腾的石头和真空蒸馏在残余的二氯甲烷和水，直到它是清除那唯一的 P2P 离开。使用干净的接收器和新鲜煮石头，提取在 P2P 在 105-115癈。不去在一个温度低于 105癈浓缩提炼或 P2P 将结转污染物，污染物被较暗的颜色。P2P 是一种清晰、 淡黄色的液体，闻起来像猫尿。P2P 将自动氧化在几周内如果左在室温，所以把它放在冰箱里直到准备使用。一个可以使用甲苯 P2P 提取水中，但它必须是真空蒸馏和分离将到而不是像二氯甲烷底部顶部。它同样多的时间大约需要分离作为时使用二氯甲烷。

結果 (中文) 3:

4.4.2铁还原1-phenyl-2-nitropropene到1 -苯基-2 -丙酮

倒入15升干净的自来水进入容器。按照这个催化铁4000g，3400克（20）1-苯基- 2-nitropropene和氯化铁40 50克。装配前在回流冷凝器，启动水流过冷凝器，开始搅拌，并点燃丙烷燃烧器。看温度计和关闭的热量，当温度达到90癈。慢慢将超过2小时内小剂量盐酸。关注事物的冷凝器顶部走出手。这种反应需要在一个小棚子或其他附属建筑通风良好的执行。安装重型（500立方英尺）里的排气扇。这是因为从这个反应的气体有很强的腐蚀性，如果反应进入失控，一个将要放弃掉一段时间随着烟雾清除。添加共15升的盐酸。一旦所有的酸已被添加，使搅拌持续2个小时在进入下一步之前。

我们现在必须从反应容器内部的肮脏的黑色乱开采我们的P2P。我们将通过水蒸气蒸馏法。断开电容器，法兰，和“T”，离开2“乳头开。搅拌器应保持转动。接下来，迅速倒入4升左右的饱和碱溶液，冷却过夜。一些热蒸汽将产生碱液中和盐酸。组装三通，法兰，并在蒸馏冷凝器和水模式开始流经冷凝器。一个20升的水桶在端和点燃丙烷燃烧器高。停止搅拌。提取过水和P2P直到桶装满，然后关火。

这种减少的收益率是75%，无论多么严重的人认为他已经搞砸了，所以我们应该期望获得15颗痣，或稍微超过2000 P2P。由于P2P具有密度接近于水，这相当于约2升的产品。

我们现在必须从水P2P，提取纯化，和存储供以后使用。这是通过注入水/ P2P 3000ml分为每两个4000ml分液漏斗完成。然后增加了饱和碱液每300ml摇大力3-5分钟。这样做是为了确保没有残留的酸可以，将催化剂中毒，使用时。一个彻底的晃动之后，二氯甲烷400ml添加到每个分液漏斗，摇匀，2-3分钟。二氯甲烷是大多数塑料的易得的溶剂。检查塑料供应商店出售的桶，塑料薄板，由于二氯甲烷比水重，它将加快P2P并带到SEP漏斗的底部。这需要一些时间，但是，所以一定不能匆忙。本文作者允许分离坐了6个小时后排出的底层为一一加仑的酒瓶子，甚至更好，一个琥珀色的玻璃瓶。把广场上的塑料袋和用瓶盖和盖之间的密封。添加另一个400ml二氯甲烷，使劲地摇，让它解决了前6小时排水。这是不够好，继续下一批。完成时，应该有3-4加仑的二氯甲烷/ P2P解决方案。



现在我们将恢复我们的二氯甲烷溶剂回收和提取P2P。使用圆底容器5000ML在二氯甲烷提取从39到60癈。返回到它的容器溶剂直到只有约2000ml P2P留在船。加入滚烫的石头和真空蒸馏在二氯甲烷和水的残余，直到它是明确的，只有P2P是左。用一块干净的接收机和新鲜煮石头，提取在P2P在癈TTR105-115。不要滴落在温度低于105癈或P2P将携带污染物超过它，污染物被深色。P2P是一种透明，淡黄色液体，闻起来像猫尿。P2P将自动氧化的几个星期以后，如果放置在室温下，所以把它放在冰箱，直到准备使用。

可以使用甲苯水提取物的P2P，但它必须是真空蒸馏和分离将是顶部而不是底部像二氯甲烷。它需要大约相同的时间单独使用时
二氯甲烷。