Hello,
I am starting to make my first syntheses using this system and I have some doubts, I hope you can help me with them:
1. How long do you let the NaOH solution react with the MR? I'm leaving it for about 12 hours so the layers separate properly. Is that okay?
2. Once the top layer has been removed, I measure its pH and I always get a result of 10. Why could it be and I can't get a pH of 11-12?
3. To purify it, I first filter out any solids that may be present through a coffee filter, then I decant it using a funnel and put the resulting liquid in the refrigerator for a few hours to crystallize any impurities that may remain and eliminate them using another filter. Would this be correct? Should I subsequently evaporate the solvent? Did I leave any more steps for purification?
I hope you can help me with this, on the other hand I would like to know if to make, for example, 300 g of P2PNP, it is mandatory to make the amalgam with 30 L of water or this amount of water could be reduced in the reaction. With the IPA and the GAA, should I also use 3 and 1.5 L respectively or could these quantities be reduced?
I am starting to make my first syntheses using this system and I have some doubts, I hope you can help me with them:
1. How long do you let the NaOH solution react with the MR? I'm leaving it for about 12 hours so the layers separate properly. Is that okay?
2. Once the top layer has been removed, I measure its pH and I always get a result of 10. Why could it be and I can't get a pH of 11-12?
3. To purify it, I first filter out any solids that may be present through a coffee filter, then I decant it using a funnel and put the resulting liquid in the refrigerator for a few hours to crystallize any impurities that may remain and eliminate them using another filter. Would this be correct? Should I subsequently evaporate the solvent? Did I leave any more steps for purification?
I hope you can help me with this, on the other hand I would like to know if to make, for example, 300 g of P2PNP, it is mandatory to make the amalgam with 30 L of water or this amount of water could be reduced in the reaction. With the IPA and the GAA, should I also use 3 and 1.5 L respectively or could these quantities be reduced?
You prepare a solution of sodium hydroxide in water in advance, so that the mixture has time to cool down (the reaction is exothermic when mixed with water). Using a cool hydroxide solution would be the most correct. The reaction with the reaction mixture should proceed quite quickly if all the aluminum has reacted or the residue has been filtered off. Then, the separation of the base occurs instantaneously after mixing with the required amount of hydroxide solution (but we add it gradually, of course).
A basic pH of 10 or greater is sufficient for base separation.
You need to distill off the solvent if you have an excess left after the reaction – if it’s an alcohol, it hinders crystallization without adding excess acetone.
The proportions are preferably maintained when scaling up, but the 300g reaction is quite specific and requires a disproportionate increase in reaction volume and certain experience to control the reaction. Furthermore, the yield is usually lower than when making smaller batches. This can be corrected, but it requires equipment.
A basic pH of 10 or greater is sufficient for base separation.
You need to distill off the solvent if you have an excess left after the reaction – if it’s an alcohol, it hinders crystallization without adding excess acetone.
The proportions are preferably maintained when scaling up, but the 300g reaction is quite specific and requires a disproportionate increase in reaction volume and certain experience to control the reaction. Furthermore, the yield is usually lower than when making smaller batches. This can be corrected, but it requires equipment.
At least to room temperature. It can be cooled further, but so as not to get sodium hydroxide crystallization back.
Distillation of the solvent is not always necessary. You can apply this if you have problems with crystallization. Or if you want to obtain pure a-oil for transportation. However, for such distillation, it is desirable to dry the solution to avoid losing the base due to the distillation of water particles. Then, use vacuum distillation for better and faster separation. If necessary for purity, the base itself can be distilled.
Approximately 50g of NaOH is usually sufficient for 10g of P2NP. Otherwise, the quantity will vary depending on the reaction mixture, residual aluminum, and so on.
For pure base without solvents, crystallization is possible when lowering the temperature (below the melting point).
Distillation of the solvent is not always necessary. You can apply this if you have problems with crystallization. Or if you want to obtain pure a-oil for transportation. However, for such distillation, it is desirable to dry the solution to avoid losing the base due to the distillation of water particles. Then, use vacuum distillation for better and faster separation. If necessary for purity, the base itself can be distilled.
Approximately 50g of NaOH is usually sufficient for 10g of P2NP. Otherwise, the quantity will vary depending on the reaction mixture, residual aluminum, and so on.
For pure base without solvents, crystallization is possible when lowering the temperature (below the melting point).