Hello, using this procedure you can get 50% d isomer and 50% l isomer for the first time. The procedure is 1g of free base / 1g of tartaric acid / 2 ml of water.
Prepare the steam-distilled free base (after steam distillation, the free base can be separated without solvent extraction and used straight away. Save the lower part, which contains most of the water, because there is still some amount of free base in it, if there is a lot of it, you can extract it, dry it and evaporate the solvent you get the rest of what is left there). Now pour into a beaker or where you want, for example, 100g of tartaric acid, add 200ml of water to it. Stir until the powder dissolves. When this happens, pour in the free base, in a few seconds or minutes you will see a thick mass that is tartrate. Now a very important point is when the mass is solid, so you have to heat it and stir it until everything dissolves, the liquid must remain completely clear. If you do it in a beaker, put a glass plate on top so that the water does not evaporate, it will smoke a little. It will not be necessary to heat until boiling, I have never measured the temperature, but it is simply necessary that everything dissolves completely, it is not enough that the liquid is milky, it must be completely transparent and look like distilled water. Then put the top down, cover it with something, for example food foil, so that it does not evaporate, and leave it somewhere to cool without moving. The minimum time needed is 4 hours, nothing will happen to it even if you leave it for 20 hours, it must be cold and precipitated long needle crystals of tartrate. When this happens when you are preparing a buchner vacuum filter or a centrifuge or whatever you like, you break the hard crystals of tartrate and filter it. In water, you will have the desired d isomer and in solid tartrate the l isomer.You just add sodium hydroxide 30% to the liquid until the pH is 13, add toulen or some other solvent to extract and then titrate the solvent. Now you can quickly evaporate the water part, then scrape off the solid material, crush it into powder and recrystallize it in 50% ethanol and 50% water. You add powdered alcohol from water until crystals start to appear on the surface of the liquid at the boiling temperature, at this point you put the recrystallization container down from the heater, cover it with something so that it does not evaporate, wait a few hours, usually about 5-6 hours are enough, it depends on whether you have thickened the liquid enough with the material, then you put the container in the freezer for a few minutes, about 30 minutes, it depends if you have not evaporated a lot of alcohol so that the liquid does not freeze in the freezer, it is only a matter of cooling down, now we just tip the crystals out of the crystallization container into the bucherovno or whatever you want and we have a finished product. We thicken the liquid that you suck out of the crystals and let them crystallize again. You can still dry the crystals with a heat gun for hair if they seem wet. You'll thank me later. I am asking all people to share the procedures that you know are good.
There is no need to washing off this tartar, even without it you will be more than satisfied with the result. When washing with water or ice-dry methanol was tried, it never helped, only a racemate-like product was obtained from the washing. Tartaric acid CAS 87-69-4 was used. After heating, let the liquid cool down at room temperature, that is the right temperature for filtering
Prepare the steam-distilled free base (after steam distillation, the free base can be separated without solvent extraction and used straight away. Save the lower part, which contains most of the water, because there is still some amount of free base in it, if there is a lot of it, you can extract it, dry it and evaporate the solvent you get the rest of what is left there). Now pour into a beaker or where you want, for example, 100g of tartaric acid, add 200ml of water to it. Stir until the powder dissolves. When this happens, pour in the free base, in a few seconds or minutes you will see a thick mass that is tartrate. Now a very important point is when the mass is solid, so you have to heat it and stir it until everything dissolves, the liquid must remain completely clear. If you do it in a beaker, put a glass plate on top so that the water does not evaporate, it will smoke a little. It will not be necessary to heat until boiling, I have never measured the temperature, but it is simply necessary that everything dissolves completely, it is not enough that the liquid is milky, it must be completely transparent and look like distilled water. Then put the top down, cover it with something, for example food foil, so that it does not evaporate, and leave it somewhere to cool without moving. The minimum time needed is 4 hours, nothing will happen to it even if you leave it for 20 hours, it must be cold and precipitated long needle crystals of tartrate. When this happens when you are preparing a buchner vacuum filter or a centrifuge or whatever you like, you break the hard crystals of tartrate and filter it. In water, you will have the desired d isomer and in solid tartrate the l isomer.You just add sodium hydroxide 30% to the liquid until the pH is 13, add toulen or some other solvent to extract and then titrate the solvent. Now you can quickly evaporate the water part, then scrape off the solid material, crush it into powder and recrystallize it in 50% ethanol and 50% water. You add powdered alcohol from water until crystals start to appear on the surface of the liquid at the boiling temperature, at this point you put the recrystallization container down from the heater, cover it with something so that it does not evaporate, wait a few hours, usually about 5-6 hours are enough, it depends on whether you have thickened the liquid enough with the material, then you put the container in the freezer for a few minutes, about 30 minutes, it depends if you have not evaporated a lot of alcohol so that the liquid does not freeze in the freezer, it is only a matter of cooling down, now we just tip the crystals out of the crystallization container into the bucherovno or whatever you want and we have a finished product. We thicken the liquid that you suck out of the crystals and let them crystallize again. You can still dry the crystals with a heat gun for hair if they seem wet. You'll thank me later. I am asking all people to share the procedures that you know are good.
There is no need to washing off this tartar, even without it you will be more than satisfied with the result. When washing with water or ice-dry methanol was tried, it never helped, only a racemate-like product was obtained from the washing. Tartaric acid CAS 87-69-4 was used. After heating, let the liquid cool down at room temperature, that is the right temperature for filtering
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