Recrystallisation of 5-methoxy-n,n-dimethyltryptamine (5-meo-dmt)
AssigneeGh Research Ireland Limited
InventorsLeonard Gerard Francis Patrick, Shaun Neil Robinson, Theis Terwey
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Abstract
A method of purifying 5-methoxy-N,N-dimethyltryptamine (5-MeO-DMT) is provided which comprises dissolving crude 5-MeO-DMT in a solvent at a temperature above room temperature, cooling the obtained solution to a temperature below room temperature to precipitate solid 5-MeO-DMT, separating the solid 5-MeO-DMT from the remaining solution and removing solvent from the crystalline 5-MeO-DMT. In the method, the solvent comprises one or more ethers and less than 5 wt % anti-solvent.
Claims18
Method of purifying 5-methoxy-N,N-dimethyltryptamine (5-MeO-DMT) comprising
- dissolving crude 5-MeO-DMT in a solvent at a temperature above room temperature
- cooling the obtained solution to a temperature below room temperature to precipitate solid 5-MeO-DMT
- separating the solid 5-MeO-DMT from the remaining solution
- removing solvent from the crystalline 5-MeO-DMT
- wherein the solvent comprises one or more ethers and less than 5 wt % of aliphatic hydrocarbons as anti-solvents.
Method according to any of the preceding claims, wherein the recrystallisation solvent contains at least 50 wt %, preferably at least 70 wt % and in particular at least 90 wt % of one or more ethers.
Method according to any of the preceding claims, wherein the recrystallisation solvent contains less than 2 wt % aliphatic hydrocarbons.
Method according to any of the preceding claims, wherein the recrystallisation solvent contains at least 98 wt % MTBE.
Method according to any of the preceding claims, wherein the solvent comprises less than 5 wt % in total of any anti-solvents, wherein anti-solvent means a liquid in which the solubility of 5-MeO-DMT at any temperature occurring during the recrystallisation is less than 20% the solubility in the ether used, or, in case that more than one ether is used, in the combination of ethers present in the dissolution solvent.
Method according to any of the preceding claims, wherein the solution is cooled to a temperature in the range of 0 to 20° C.
Method according to any of the preceding claims additionally comprising a step of reducing the amount of remaining recrystallisation solvent.
Method according to any of the preceding claims, wherein the total amount of impurities is reduced to below 0.5 area % as determined by HPLC using UV detection at 227 nm and/or wherein the amount of each individual impurity is reduced to below 0.1 area % as determined by HPLC using UV detection at 227 nm.
5-Methoxy-N,N-dimethyltryptamine (5-MeO-DMT), wherein the total amount of impurities is below 0.5 area % and wherein the amount of each individual impurity is below 0.1 area %, wherein the amounts of impurities are determined by HPLC carried out with an octadecyl carbon chain-bonded silica (C18) column and a mixed solvent based on 0.013M ammonium acetate in water and acetonitrile as eluent, using UV detection at 227 nm.
Dependencies are inferred from the claim text.