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OK, so I've had a little play around with 2.1 grams of decidedly damp freebase harmalas from the PC cooks with ascorbic acid based with ammonia. They were still damp after washes with 5% ammonia.

8 pulls with c. 20 mL BuOAc each time making a total of 150 mL of a yellow-coloured extract which fluoresces blue! All the pulls from start to finish fluoresced the same shade of blue, and the remaining solids have lost their reddish cast, going from kind of somewhat reddish cigar brown to a much darker shade. The fluorescence contrasts markedly with the green of an aqueous solution of the mixed harmala ascorbate.

It got to the point where I had to stop work for the night so it still remains to be seen whether the remaining solids will dissolve if further fractions of BuOAc are used. Also on the cards is checking what colour fluorescence the residual solid might produce when dissolved in either more solvent and/or in acid.

There was no time to try out a citric acid precipitation yet. Firstly, the final pull of the wash is still settling; the remaining solid had become completely powdery after starting out as a paste. This indicates that the butyl acetate does incrementally dissolve out the water in small amounts. The solvent was dried by swirling over sodium chloride crystals before use to assist this process of drying out the paste, although initially the solvent was used as it came and instead the first 3 pulls were removed and dried half way through the process and then returned to the paste.

One observation with the first few (~4) pulls was that the paste became more liquid as the more soluble harmala base dissolved out more quickly than the water, leaving less solid in the paste. By the sixth pull, the paste started to become crumbly and on the seventh it was a clumpy powder. Separation was quick and easy with all these pulls. Only on the eighth pull had the solids become so dry that fine powder dispersed into the solvent, hence requiring an overnight settling period.

Instead of doing a preliminary citric acid precipitation test, I clumsily dropped the beaker containing the remaining 80+ grams of harmala paste onto the stone floor. After a lengthy string of expletives, I was greatly relieved that I hadn't bothered to dry out the paste as this meant that most of it remained in one large blob in a bigger fragment of beaker and the rest of it was confined to a few smaller pieces which were easy to recover with minimal losses. All of the blobs, shards and fragments were placed into a larger beaker and doused with dilute acetic acid.

The harmala acetates solution will be filtered and processed in due course. This was something I'd been meaning to do for several weeks but it was all too easy just to keep chipping away at the nice big blob of yummy alkaloids, so now my hand has been forced and this whole mishap may be considered to have progress as a silver lining

<blockquote data-quote="downwardsfromzero" data-source="post: 3886269" data-attributes="member: 1025">OK, so I&#039;ve had a little play around with 2.1 grams of decidedly damp freebase harmalas from the PC cooks with ascorbic acid based with ammonia. They were still damp after washes with 5% ammonia.8 pulls with c. 20 mL BuOAc each time making a total of 150 mL of a yellow-coloured extract which fluoresces blue! All the pulls from start to finish fluoresced the same shade of blue, and the remaining solids have lost their reddish cast, going from kind of somewhat reddish cigar brown to a much darker shade. The fluorescence contrasts markedly with the green of an aqueous solution of the mixed harmala ascorbate.It got to the point where I had to stop work for the night so it still remains to be seen whether the remaining solids will dissolve if further fractions of BuOAc are used. Also on the cards is checking what colour fluorescence the residual solid might produce when dissolved in either more solvent and/or in acid.There was no time to try out a citric acid precipitation yet. Firstly, the final pull of the wash is still settling; the remaining solid had become completely powdery after starting out as a paste. This indicates that the butyl acetate does incrementally dissolve out the water in small amounts. The solvent was dried by swirling over sodium chloride crystals before use to assist this process of drying out the paste, although initially the solvent was used as it came and instead the first 3 pulls were removed and dried half way through the process and then returned to the paste.One observation with the first few (~4) pulls was that the paste became more liquid as the more soluble harmala base dissolved out more quickly than the water, leaving less solid in the paste. By the sixth pull, the paste started to become crumbly and on the seventh it was a clumpy powder. Separation was quick and easy with all these pulls. Only on the eighth pull had the solids become so dry that fine powder dispersed into the solvent, hence requiring an overnight settling period.Instead of doing a preliminary citric acid precipitation test, I clumsily dropped the beaker containing the remaining 80+ grams of harmala paste onto the stone floor. After a lengthy string of expletives, I was greatly relieved that I hadn&#039;t bothered to dry out the paste as this meant that most of it remained in one large blob in a bigger fragment of beaker and the rest of it was confined to a few smaller pieces which were easy to recover with minimal losses. All of the blobs, shards and fragments were placed into a larger beaker and doused with dilute acetic acid.The harmala acetates solution will be filtered and processed in due course. This was something I&#039;d been meaning to do for several weeks but it was all too easy just to keep chipping away at the nice big blob of yummy alkaloids, so now my hand has been forced and this whole mishap may be considered to have progress as a silver lining <img src="data:image/gif;base64,R0lGODlhAQABAIAAAAAAAP///yH5BAEAAAAALAAAAAABAAEAAAIBRAA7" class="smilie smilie--sprite smilie--sprite8" alt=":D" title="Big grin&nbsp; &nbsp; :D" loading="lazy" data-shortname=":D" /></blockquote>

[QUOTE="downwardsfromzero, post: 3886269, member: 1025"] OK, so I've had a little play around with 2.1 grams of decidedly damp freebase harmalas from the PC cooks with ascorbic acid based with ammonia. They were still damp after washes with 5% ammonia. 8 pulls with c. 20 mL BuOAc each time making a total of 150 mL of a yellow-coloured extract which [b]fluoresces blue[/b]! All the pulls from start to finish fluoresced the same shade of blue, and the remaining solids have lost their reddish cast, going from kind of somewhat reddish cigar brown to a much darker shade. The fluorescence contrasts markedly with the green of an aqueous solution of the mixed harmala ascorbate. It got to the point where I had to stop work for the night so it still remains to be seen whether the remaining solids will dissolve if further fractions of BuOAc are used. Also on the cards is checking what colour fluorescence the residual solid might produce when dissolved in either more solvent and/or in acid. There was no time to try out a citric acid precipitation yet. Firstly, the final pull of the wash is still settling; the remaining solid had become completely powdery after starting out as a paste. This indicates that the butyl acetate does incrementally dissolve out the water in small amounts. The solvent was dried by swirling over sodium chloride crystals before use to assist this process of drying out the paste, although initially the solvent was used as it came and instead the first 3 pulls were removed and dried half way through the process and then returned to the paste. One observation with the first few (~4) pulls was that the paste became more liquid as the more soluble harmala base dissolved out more quickly than the water, leaving less solid in the paste. By the sixth pull, the paste started to become crumbly and on the seventh it was a clumpy powder. Separation was quick and easy with all these pulls. Only on the eighth pull had the solids become so dry that fine powder dispersed into the solvent, hence requiring an overnight settling period. Instead of doing a preliminary citric acid precipitation test, I clumsily dropped the beaker containing the remaining 80+ grams of harmala paste onto the stone floor. After a lengthy string of expletives, I was greatly relieved that I hadn't bothered to dry out the paste as this meant that most of it remained in one large blob in a bigger fragment of beaker and the rest of it was confined to a few smaller pieces which were easy to recover with minimal losses. All of the blobs, shards and fragments were placed into a larger beaker and doused with dilute acetic acid. The harmala acetates solution will be filtered and processed in due course. This was something I'd been meaning to do for several weeks but it was all too easy just to keep chipping away at the nice big blob of yummy alkaloids, so now my hand has been forced and this whole mishap may be considered to have [i]progress[/i] as a silver lining :D [/QUOTE]