even after re-crystallization, it remained very dirty, if the video shows the usual p2np. at least recrystallize again, and even better, send the whole without purification to p2p
any alcohol will do, it has not to be only IPA. You forget the most important of all buddy, that is to wash / ruinse the P2BP crystals with sodium bisulphite after recrystallization. Whatever method you used to make the P2NP always a small ampount (0.25% up to 5%) of benzaldehyde always contaminate the crsytals of P2NP when they crash out. Sodium bisulphite 6-8% solution in water is the best and most easy way to wash out that benzaldehyde. benzaldehyde interfere in whatever reaction you had in mind for your P2NP
any alcohol will do, it has not to be only IPA. You forget the most important of all buddy, that is to wash / ruinse the P2BP crystals with sodium bisulphite after recrystallization. Whatever method you used to make the P2NP always a small ampount (0.25% up to 5%) of benzaldehyde always contaminate the crsytals of P2NP when they crash out. Sodium bisulphite 6-8% solution in water is the best and most easy way to wash out that benzaldehyde. benzaldehyde interfere in whatever reaction you had in mind for your P2NP
My technique is a bit different, I bought a 50l milk barrel, mounted 1.2kw motor on the top,with bearing and metal shaft,welded lawnmover propeler,for speed reguliator i use transformer,,and i drill hole for termometer,also bought Rex c100 thermoregulator,for elektric 3kw heatingplate,10kg p2np with 20lmetanol,you need stop motor ,open lid every 15min,and check,if melted or not,and do fast becose then you stop motor,temperature changes,(Smell is abnormal!)i can tell you is not a dream job,!Afte finish,you get very nice needles,i always do, 3 times for clear white needles.,,,box refrigerator minimum -20c no less,it last for very long period,its more stable product,compare to bmk.
Deep freezer always, at minus celsius -12 or higher frezing point, -12 to -20 is odeal, you can keep it for years like that. Always di a minimal amount of alcohol re-crysdtallization anyways when you take it out for use next time
P2NP will dissolve in Sodium bisulphite solution, but the benzaldehyde is solveble in bisuphite solution, that is the whole point of tis washin, you wash out the benzaldehyde rest from tyhe crustals, the crystals do not dfissolve in the bisuphite water solution (it will only remove the bebnzaldehyde from the crystals and leave them clean from bernzaldehyde contamination). Seperate it at the Buchner funnel and sucvk the P2NP as dry as possible, then to make crystals ultra dry from any water bry the crystals in a dessicator for 24 hrs also after the bisulphite rinssing. Then you have 99.99% dry and +99.5% pure P2NP
I took benzaldehyde 50 ml nitroethane 50 ml glacial acetic acid 13 ml n-butylamine 20 ml in a 500 ml beaker and covered the mouth of the beaker with rubber gloves. Then I heated it in the microwave oven until bubbles appeared, (40-45 seconds) and then turned it off. After heating it each time, I cooled it to room temperature. After doing this 7 times, the color of my mixture became very light yellow. The microwave oven had 700 watts. When I saw that this was not happening. Then I put the mixture under reflux. After refluxing for 3 hours, it remained light yellow. I added 1 gram of ammonium acetate during the reflux. After 2 hours, I saw a dark yellow color. Then I added another half gram of ammonium acetate. After 3 hours of addition, a dark orange color appeared. I put the mixture in a beaker and left it for 5 hours. No crystals were seen. I added cold purified water to the dark orange mixture as a washing agent. And separated the mixture with a separating funnel and washed it 3 times. To separate the mixture, I added anhydrous magnesium sulfate to that mixture and stirred it every now and then so that it could absorb the water well. After 30 minutes, I separated the magnesium sulfate by filtering it. Now I have a dark orange oil-like mixture. What should I do then? How can I make crystals from this liquid, Please tell me please help me.
I took benzaldehyde 50 ml nitroethane 50 ml glacial acetic acid 13 ml n-butylamine 20 ml in a 500 ml beaker and covered the mouth of the beaker with rubber gloves. Then I heated it in the microwave oven until bubbles appeared, (40-45 seconds) and then turned it off. After heating it each time, I cooled it to room temperature. After doing this 7 times, the color of my mixture became very light yellow. The microwave oven had 700 watts. When I saw that this was not happening. Then I put the mixture under reflux. After refluxing for 3 hours, it remained light yellow. I added 1 gram of ammonium acetate during the reflux. After 2 hours, I saw a dark yellow color. Then I added another half gram of ammonium acetate. After 3 hours of addition, a dark orange color appeared. I put the mixture in a beaker and left it for 5 hours. No crystals were seen. I added cold purified water to the dark orange mixture as a washing agent. And separated the mixture with a separating funnel and washed it 3 times. To separate the mixture, I added anhydrous magnesium sulfate to that mixture and stirred it every now and then so that it could absorb the water well. After 30 minutes, I separated the magnesium sulfate by filtering it. Now I have a dark orange oil-like mixture. What should I do then? How can I make crystals from this liquid, Please tell me please help me.
I've never done this before so I don't have any. I've tried rubbing it with a glass rod many times over the course of several days, but there are no crystals.
yo, when you finished ur irradiation did you add
200mls of 100% ipa to the rm, then covered with glad wrap and placed in the freezer.
i took a little bit of the reaction mixture and evaporated to get a seed crystal.
once i added the seed crystal, boom p2np instantly crystallized.
i then placed rm back in the freezer.
i will vacuum filter shortly and wash crystals with amount of cold ipa, then weigh crystals.
then will place motherliquour back in freezer for a second crop.
