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.
Claims15
A method of purifying 5-methoxy-N,N-dimethyltryptamine (5-MeO-DMT) comprising:
- dissolving crude 5-MeO-DMT in a recrystallisation solvent at a temperature above room temperature to obtain a solution;
- cooling the obtained solution to a temperature below room temperature to precipitate a solid, the solid comprising crystalline 5-MeO-DMT;
- separating the crystalline 5-MeO-DMT from the remaining solution;
- and
- removing the recrystallisation solvent from the crystalline 5-MeO-DMT to obtain a purified 5-MeO-DMT product;
- wherein the recrystallisation solvent contains at least 98 wt % methyl tert.-butyl ether (MTBE).
A method of purifying 5-methoxy-N,N-dimethyltryptamine (5-MeO-DMT) comprising:
- dissolving crude 5-MeO-DMT in a recrystallisation solvent at a temperature above room temperature to form a mother liquor, wherein the crude 5-MeO-DMT contains a total amount of impurities of 0.5 area % to 5 area %, based on peak area in an HPLC chromatogram;
- cooling the mother liquor to a temperature below room temperature to precipitate a solid, the solid comprising crystalline 5-MeO-DMT;
- separating the crystalline 5-MeO-DMT from the mother liquor;
- and
- after the separation of the crystalline 5-MeO-DMT from the mother liquor, removing any remaining recrystallisation solvent from the crystalline 5-MeO-DMT to obtain a crystalline 5-MeO-DMT product in which the total amount of impurities in the crystalline 5-MeO-DMT product is below 0.5 area % and the amount of each individual impurity is below 0.1 area %;
- wherein
- the recrystallisation solvent contains at least 98 wt % methyl tert.-butyl ether (MTBE), and
- the crystalline 5-MeO-DMT product is generated from the crude 5-MeO-DMT without performing column chromatography.
A method of purifying 5-methoxy-N,N-dimethyltryptamine (5-MeO-DMT) comprising:
- dissolving crude 5-MeO-DMT in a recrystallisation solvent at a temperature above room temperature to obtain a solution;
- performing a recrystallization by cooling the obtained solution to a temperature below room temperature to precipitate a solid, the solid comprising crystalline 5-MeO-DMT;
- separating the crystalline 5-MeO-DMT from the remaining solution;
- and
- removing the recrystallisation solvent from the crystalline 5-MeO-DMT to obtain a purified 5-MeO-DMT product in which an amount of each individual impurity in the purified 5-MeO-DMT product is below 0.1 area %, the amount of each individual impurity being 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;
- wherein
- the recrystallisation solvent contains at least 98 wt % methyl tert.-butyl ether (MTBE), and
- the purified 5-MeO-DMT product is obtained by performing the recrystallization only once.
Dependencies are inferred from the claim text.