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> how to make lsd
> making lsd from lysergic acid
below is a detailed method of making lsd from chemicals. it should be noted that this file is for informational purposes and that incorrectly following these instructions could be harmful or fatal. the proprietors of this website makes no claims as to the safety of the following prodecure and places it here for educational pruposes only. under no circumstances should anyone try this.
dissolve 13.4g dry (i) in 250 ml dry dimethformamide and cool to 0¡c. add cooled solution of 3.4 ml 0.35 m methanesulfonic acid anhydride in dry dimethylformamide. after thirty minutes at 0¡c add 14.6g (20.4 ml) diethylamine (dea) and keep at 0¡c for one hour. evaporate in vacuum to get lsd.
dissolve 5.3g dry (i) in 125 ml acentonitrile (or dimethylformamide or proprionitrile) and cool to -20¡c (freezer or dry ice-acetone or ethanol mixture). add 8.82g trifluroacetic anhydride in 75 ml acetonitrile cooled to -20¡c carefully. let stand at - 20 for 1 1/2 hours or until all (i) dissolves. then add 7.6g dea in 150ml acetonitrile and let stand at room temperature in dark two hours. evaporate in vacuum to get lsd.
dissolve 0.536g (i) in 10 ml freshly distilled pocl3; stir and add 416mg powdered, freshly sublimed pcl5. hold two minutes at room temperature, two minutes at 90¡c, and evaporate in vacuum. extract the residue with hexane to give the lysergic acid chlo ride-hcl (can also extract the reaction mixture with hexane instead of evaporating in vacuum). alternatively use 6ml pocl3 and 240 mg socl2 and heat three minutes at 90¡c to get the acid chloride. to 5g of the acid chloride add 1.4ml dea in 50ml methane c hloride and cool to 0¡c. stir and add 27.5 ml pyridine and stir 1/2 hour at 0¡ . warm to room temperature and stir 1 1/2 hours. evaporate in vacuum to get lsd.
to a suspension of 13.4g dry (i) in 800ml dry dimethylformamide (dmf) in a 2l vacuum flask at 20¡, add a solution of 8.9g n,n'-carbonyldiimidazole in 250ml dmf and stir at 20¡ in dark for 1/2 hour. add a solution of 4g dea in 50ml dmf and let stand 2 hou rs at 20¡;then purify or dissolve residue in 2 1/2l 2% tartaric acid; nh4oh and extract with a 9:1 solution of ether:ethanol. dry and evaporate in vacuum to get lsd.
add 1l dimethylformamide (freshly distilled if possible) to dry flask fitted with stirrer, ice bath, dropping funnel and condenser, both protected from water by ca chloride drying tubes. add dropwise with stirring over 4-5 hours at 0¡ 0.21bs (90.7g) so 3 (sulfuric anhydride, available as sulfan from allied chem co.) if precipitate forms, stir until it dissolves. sulfan may be made in larger amounts and is good for several months if kept dry and cool. molarity of fresh so3-dmf reagant should be about 1m, but for precise determination add a little water to aliquot and titrate with standard naoh to phenolphthalein end point. add 6.45g dry (i) (or 7.15g (i) monohydrate) and 1.06 lioh hydrate to 200ml methanolin a 1l vacuum flask and evaporate in vacuum. dis olve residue in 400ml dmf at about 15mm hg through a twelve inch column packed with glass helices or other material. cool to 0¡ and rapidly add 50ml so3-dmf solution (1 m). stir at 0¡ for ten minutes and add 91.5g (12.9ml) dea and stir ten minutes. add 400ml water, stir and add 200ml saturated nacl. extract the lsd by shaking with several 500ml portions ethylene dichloride (can use indole test to show completeness of extraction). combine extracts (lower layor in seporatory funnel) and dry, evaporate in vacuum to get lsd.
to a reflexing slurry of 3.15g dry (i)(or monohydrate) in 150ml chcl3 add 0.1 mole of the amine in 25ml chcl3 and 2ml pocl3 simultaneously from seperate dropping funnels over 2 to 3 minutes. reflux 3 to 5 minutes more till a clear amber solution result s. cool to room temperature and wash with 200ml 1m nh4oh. dry and evaporate in vacuum(below 40¡c). can dissolve in the minumum amount of methanol. filter and wash crystals with cold methanol and acidify with a fresh solution of 20% maleic acid in methanol . filter and wash crystals with cold methanol to get the lsd or other amide. this method works with a wide variety of amines. for lsd itself, the pocl3 can be added first. the yield is about 50%.
to purify your extracted lsd dissolve the residue in 150ml chcl3 and add 20ml ice water. pour into 1/2l seperatory funnel and drain out the lower chcl3 layer into a beaker (after shaking). add 50ml chcl3 to funnel, shake and drain bottom layer into same beaker. repeat with 3 x 50ml chcl3 and discard the water. extract the combined chcl3 extracts with 4 x 50ml ice cold water and dry, evaporate in vacuum the chcl3 to get 3.5g d-lsd. this is composed partly of inactive d-iso-lsd which can be recovered and c onverted to d-lsd as follows: dissolve the residue in 120ml benzene and 40ml chcl3 (or 200ml methanol), add tartaric or maleic acid and shake to precipitate mainly d-lsd (add a little ether and cool in refrigerator several days if nessecary to ensure comp lete precipitation)) evaporate in vacuum the solvent to get d-iso-lsd. ad 50ml ethanol and 5ml 4n koh per g iso-lsd and let stand at room temperature for two hours, evaporate in vacuum (or extract with chcl3 as above) to get lsd.
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