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Following the inconclusive/incomplete information I had previously posted in this thread, here is a full write-up of this procedure.

An alkaloid extract of the Thoughtful Tree was isolated by standard A/B extraction, the details of which are commonly spread throughout this forum. The solvent used was hexane isomers with some pentane and cyclohexane as adulterants. Works just like naphtha for freeze-precipitation, hereafter referred to simply as hexanes. The extract is very gooey.

3 grams of this extract was added to a small beaker. To this was added the minimum amount of dry methanol at 27°C and stirred until it all dissolved. To another beaker was added 12x 325mg tablets of aspirin. These were crushed to a powder and the minimum amount of methanol was added and stirred to dissolution. The solution was filtered and the filter was washed with a little more methanol. These two solutions were combined in a flat-bottomed flask. The total volume at this point was 60-70 ml.

The flask was then heated in a 55°C water bath until methanol vapor evolved. This took about 10 minutes. The temp was held at 55°C for another 10 minutes. The flask was then cooled under running cold water until the liquid was at 20°C. About 50ml 31% HCl was diluted with water to an approximate volume of 220 ml. This was added to the cooled methanol solution resulting in a volume of 300ml. This was extracted with 3x 45 ml DCM, which turned yellow on the first extraction. The combined DCM was back-extracted with a small amount of HCl (about 45 ml). The combined aqueous layer had some junk floating around in it so it was filtered, resulting in a nice (disappointingly) clean looking aqueous solution.

The aqueous layer was basified slowly with concentrated NaOH until the cloudiness did not dissipate upon mixing. pH was measured at around 14. This solution, while at around 40°C, was extracted with 2x 75ml hexanes. This 150 ml hexanes solution was filtered and placed in the freezer. Crystallization immediately commenced, and results will be posted tomorrow.

The combined DCM solution was filtered and distilled leaving a very clean-looking white crystalline residue in the distilling flask. This was removed with acetone, and the acetone was evaporated on a steam bath with a fan, resulting in a white to slightly hi-liter yellow crystalline material.

There is 3.3g of this material, which I take to be a mixture of salicylic acid, acetylsalicylic acid, and N-methyl-N-acetyltryptamine. Its smell is both sour and tryptamine-like. It is soluble in DCM and acetone. A component of this mixture crystallizes from acetone similarly to DMT, with circular needle-like formations. Melting point is obviously much greater than 88°C, as at this temperature there is no hint of softening or melting.

It would be interesting if anyone had any information about N-methyl-N-acetyltryptamine. Likely a hydrolysis will be attempted and reported.

RESULT: 2.2g of the Good Stuff!
Upon collection and drying of the precipitated output of this procedure, it weighs in at 2.2g which is considerably more than I expected. The color of this material is blindingly white, and it is a bit waxy and slightly oily. It would appear that this material still contains some NMT, based on its texture being more waxy than crispy. The aroma is still a bit muted. Bioassay indicates however that everything is wonderful.

I think the next attempt at this procedure will feature a reflux in the alcohol so that temperature can be maintained longer. I am definitely happy with the result. It was easy to load into the pipe, and it had a pronounced and hard-hitting effect. The flavor is like MHRB extract only a little softer. Next time I try this I'll report on whether the refluxing has any effect.

<blockquote data-quote="lysurgeon" data-source="post: 3601424" data-attributes="member: 3336">Following the inconclusive/incomplete information I had previously posted in this thread, here is a full write-up of this procedure.&nbsp; An alkaloid extract of the Thoughtful Tree was isolated by standard A/B extraction, the details of which are commonly spread throughout this forum.&nbsp; The solvent used was hexane isomers with some pentane and cyclohexane as adulterants.&nbsp; Works just like naphtha for freeze-precipitation, hereafter referred to simply as hexanes.&nbsp; The extract is very gooey.3 grams of this extract was added to a small beaker.&nbsp; To this was added the minimum amount of dry methanol at 27°C and stirred until it all dissolved.&nbsp; To another beaker was added 12x 325mg tablets of aspirin.&nbsp; These were crushed to a powder and the minimum amount of methanol was added and stirred to dissolution.&nbsp; The solution was filtered and the filter was washed with a little more methanol.&nbsp; These two solutions were combined in a flat-bottomed flask.&nbsp; The total volume at this point was 60-70 ml.The flask was then heated in a 55°C water bath until methanol vapor evolved.&nbsp; This took about 10 minutes.&nbsp; The temp was held at 55°C for another 10 minutes.&nbsp; The flask was then cooled under running cold water until the liquid was at 20°C.&nbsp; About 50ml 31% HCl was diluted with water to an approximate volume of 220 ml.&nbsp; This was added to the cooled methanol solution resulting in a volume of 300ml.&nbsp; This was extracted with 3x 45 ml DCM, which turned yellow on the first extraction.&nbsp; The combined DCM was back-extracted with a small amount of HCl (about 45 ml).&nbsp; The combined aqueous layer had some junk floating around in it so it was filtered, resulting in a nice (disappointingly) clean looking aqueous solution.The aqueous layer was basified slowly with concentrated NaOH until the cloudiness did not dissipate upon mixing.&nbsp; pH was measured at around 14.&nbsp; This solution, while at around 40°C, was extracted with 2x 75ml hexanes.&nbsp; This 150 ml hexanes solution was filtered and placed in the freezer.&nbsp; Crystallization immediately commenced, and results will be posted tomorrow.The combined DCM solution was filtered and distilled leaving a very clean-looking white crystalline residue in the distilling flask.&nbsp; This was removed with acetone, and the acetone was evaporated on a steam bath with a fan, resulting in a white to slightly hi-liter yellow crystalline material.There is 3.3g of this material, which I take to be a mixture of salicylic acid, acetylsalicylic acid, and N-methyl-N-acetyltryptamine.&nbsp; Its smell is both sour and tryptamine-like.&nbsp; It is soluble in DCM and acetone.&nbsp; A component of this mixture crystallizes from acetone similarly to DMT, with circular needle-like formations.&nbsp; Melting point is obviously much greater than 88°C, as at this temperature there is no hint of softening or melting.It would be interesting if anyone had any information about N-methyl-N-acetyltryptamine.&nbsp; Likely a hydrolysis will be attempted and reported.&nbsp; RESULT: 2.2g of the Good Stuff!Upon collection and drying of the precipitated output of this procedure, it weighs in at 2.2g which is considerably more than I expected.&nbsp; The color of this material is blindingly white, and it is a bit waxy and slightly oily.&nbsp; It would appear that this material still contains some NMT, based on its texture being more waxy than crispy.&nbsp; The aroma is still a bit muted.&nbsp; Bioassay indicates however that everything is wonderful.I think the next attempt at this procedure will feature a reflux in the alcohol so that temperature can be maintained longer.&nbsp; I am definitely happy with the result.&nbsp; It was easy to load into the pipe, and it had a pronounced and hard-hitting effect.&nbsp; The flavor is like MHRB extract only a little softer.&nbsp;&nbsp; Next time I try this I&#039;ll report on whether the refluxing has any effect.</blockquote>

[QUOTE="lysurgeon, post: 3601424, member: 3336"] Following the inconclusive/incomplete information I had previously posted in this thread, here is a full write-up of this procedure. An alkaloid extract of the Thoughtful Tree was isolated by standard A/B extraction, the details of which are commonly spread throughout this forum. The solvent used was hexane isomers with some pentane and cyclohexane as adulterants. Works just like naphtha for freeze-precipitation, hereafter referred to simply as hexanes. The extract is very gooey. 3 grams of this extract was added to a small beaker. To this was added the minimum amount of dry methanol at 27°C and stirred until it all dissolved. To another beaker was added 12x 325mg tablets of aspirin. These were crushed to a powder and the minimum amount of methanol was added and stirred to dissolution. The solution was filtered and the filter was washed with a little more methanol. These two solutions were combined in a flat-bottomed flask. The total volume at this point was 60-70 ml. The flask was then heated in a 55°C water bath until methanol vapor evolved. This took about 10 minutes. The temp was held at 55°C for another 10 minutes. The flask was then cooled under running cold water until the liquid was at 20°C. About 50ml 31% HCl was diluted with water to an approximate volume of 220 ml. This was added to the cooled methanol solution resulting in a volume of 300ml. This was extracted with 3x 45 ml DCM, which turned yellow on the first extraction. The combined DCM was back-extracted with a small amount of HCl (about 45 ml). The combined aqueous layer had some junk floating around in it so it was filtered, resulting in a nice (disappointingly) clean looking aqueous solution. The aqueous layer was basified slowly with concentrated NaOH until the cloudiness did not dissipate upon mixing. pH was measured at around 14. This solution, while at around 40°C, was extracted with 2x 75ml hexanes. This 150 ml hexanes solution was filtered and placed in the freezer. Crystallization immediately commenced, and results will be posted tomorrow. The combined DCM solution was filtered and distilled leaving a very clean-looking white crystalline residue in the distilling flask. This was removed with acetone, and the acetone was evaporated on a steam bath with a fan, resulting in a white to slightly hi-liter yellow crystalline material. There is 3.3g of this material, which I take to be a mixture of salicylic acid, acetylsalicylic acid, and N-methyl-N-acetyltryptamine. Its smell is both sour and tryptamine-like. It is soluble in DCM and acetone. A component of this mixture crystallizes from acetone similarly to DMT, with circular needle-like formations. Melting point is obviously much greater than 88°C, as at this temperature there is no hint of softening or melting. It would be interesting if anyone had any information about N-methyl-N-acetyltryptamine. Likely a hydrolysis will be attempted and reported. RESULT: 2.2g of the Good Stuff! Upon collection and drying of the precipitated output of this procedure, it weighs in at 2.2g which is considerably more than I expected. The color of this material is blindingly white, and it is a bit waxy and slightly oily. It would appear that this material still contains some NMT, based on its texture being more waxy than crispy. The aroma is still a bit muted. Bioassay indicates however that everything is wonderful. I think the next attempt at this procedure will feature a reflux in the alcohol so that temperature can be maintained longer. I am definitely happy with the result. It was easy to load into the pipe, and it had a pronounced and hard-hitting effect. The flavor is like MHRB extract only a little softer. Next time I try this I'll report on whether the refluxing has any effect. [/QUOTE]