ine base, as is chloroform (the dichlor can be bought online easily enough and isn't expensive. Low boiling point so avoids having to subject morphine base to excessive heat and as can chloroform although its more expensive than dichloromethane/methylene chloride and has a higher BP. It can however be made very easily using NaOCl (sodium hypochlorite, bleach, solution, along with entry level strong bases such as caustic soda and acetone and ideally distillation of the finished product after first washing the separated chloroform with water and then with saturated brine (NaCl, in hot water until reaching the solubility limit, then allowed to cool to room temperature, lowering the solubility of the same, the excess falls out of solution and then you've got yourself a saturated solution of salt, which is then used to wash the water-washed (several H2O washes first ideally to clean out the acetone, the base and hypochlorite residues etc.) a couple of times, swirling them together in a beaker (don't use plastics, chloroform as well as DCM dissolve many plastics. However high-density polyethylene resists it, and it just so happens that many modern plastic milk cartons happen to be made of HDPE (which can be found written on the bottom in that case)
Don't perform the chloroform synthesis IN the milk jugs, you want glass, because the action of sodium hydroxide on chloroform generates an extremely reactive, radical species called dichlorocarbene, and dichloromethane produces chlorocarbene, similarly reactive and will easily insert itself into all manner of organic bonds and turn plastics to slop, even if resistant to chloroform or dichlor themselves. (coincidentally, this same reaction can be exploited to test for the presence of primary amines vs secondary or tertiary amines or quaternary ammonium salts, small quantity of the suspected primary amine in dry alcohol (isopropanol is probably the easiest to get OTC, and serves here just as a solvent, its available in spray cans, very, very dry for cleaning printed circuit boards, and the electronics grade stuff is very clean, and very dry so should need no additional procedures which might be troublesome to somebody who doesn't run their own lab but just needs a bit of kitchen chemistry for drying alcohols which have reached their azeotropic concentration with H2O, beyond which all that distills off is the azeotrope, such as 95% ethanol 5% water in the case of the most commonly drunk alcohol (prefer tert-pentanol myself then first predrying over baked epsom salts, roasted in the oven at max temp with the door opened a crack to let the water vapor escape, and then some of this once cooled, kept in the oven whilst doing so to avoid hydrating in the atmospheric moisture, and once this has been done, decanting/filtering off the epsom salts
(which can be reused for this ad infinitum just bake em out again) and then treatment with first quicklime (calcium oxide) and distillation, with a drying tube packed with CaO or anhydrous CaCl2 on top of the condenser of the still-pot and any other open-to-atmosphere glass joints, collecting the distillate and then treating this with calcium carbide, which decomposes in the presence of water to give acetylene gas, which can be driven off by purging it with a stream of dry argon or nitrogen gas, available at welder's stores in small portable tanks along with the correct regulators for these disposable tanks, not that dear, the regulator will last you indefinitely and the tanks...well depends how much you need, as to how pricy, I go through bloody loads of the things, and tend to keep at least 5-6 or so spare argon tanks for my inert gas needs. In either case the calcium oxide should be added slowly, in portions, because the hydration to calcium hydroxide, Ca(OH)2 is very exothermic and in the case of acetylene you want to do it with good ventilation because it isn't great stuff to breathe, and it smells nasty. Plus commercial tech grade calcium carbide contains some proportion of phosphides which release phosphine gas, PH3, the phosphorus analog of ammonia, which is NH3, but unlike the merely irritant and when very concentrated, corrosive, or as an anhydrous cryogenic liquefied gas then it presents both a corrosive and a freeze-burn hazard since it liquefies at a little short of -40 degrees 'C IIRC) with phosphine gas, its infinitely more dangerous than ammonia, in fact its fucking lethal stuff. Stinks something nasty, fishy kind of smell, and VERY poisonous. So better buy decent grade CaC2 (calcium carbide) to minimize phosphine release, and do this outside on a portable bench)
And then once added a solution (1cc or so) of a little bit of the suspected primary amine in a dry alcohol to a mixture of potassium hydroxide solution in an alcohol (KOH is available online mainly for soapmaking, as potassium soaps tend to be liquid, or at least softer than the corresponding soaps made from saponification of fats using sodium hydroxide), 2cc of this, adding the KOH to the alcohol (wearing goggles, you do not want caustic potash in your eyes, and some latex gloves, kitchen gloves etc. just to avoid it splashing on you, if it does then just wash it off reasonably quickly with water, if in eyes irrigate the eyes copiously and if pain caused at all call an ambulance) containing a couple of drops of chloroform.
Do this OUT-FUCKING-SIDE. It relies on the production of the primary amine's corresponding isocyanide, and isocyanides can be detected by their brutal, gutwrenching, heinous abomination of a stench. I'm really, really not joking about not doing it indoors. Even with a fume-hood you won't be popular and you won't like it either. It'll stick around for days and isocyanides (otherwise known as isonitriles, or carbylamines) are not just vile, but legendary for the sheer offensiveness of the stench they pack. They just do not compare well to anything else, its difficult to describe..sweet in a rancid, putrid decay kind of sweetness way with hints of sour, again of a decaying biological material kind of way, sickly, with a vicious way of invading one's nose and forcing their way right down to your guts, tying them in a knot and kicking you in the balls from the inside repeatedly. You don't SMELL an isocyanide, it viciously commits aggravated assault upon your olfactory nerve in a primal kind of way that simultaneously tries its best to rip your stomach out and shove it up your ass, after sticking your head in a barrel of fermenting dog shit. In fact you'd gladly go and bathe in a tank of fermenting dog shit just to get the stench of isonitrile to stop attacking you.
The isocyanides generally aren't as toxic as cyanides. But the smell...by the bloody gods its the kind of atrocious filthy stink that would make you wish for cyanide poisoning instead
So the test, if positive, makes itself quite obvious with not very much of a sniff by the utterly terrible reek produced when a primary amine is present. The isocyanide test does not work with secondary or tertiary amines and afaik or on quaternary ammonium salts. It does however also work upon aromatic amines such as aniline (the result in that case would be phenyl isocyanide). The isocyanides can be destroyed once the test result is known by means of treating the sample with acid, such as hydrochloric acid (muriatic acid, spirits of salt, often used as brick cleaner) or sulfuric acid (bog unblocker of some kinds, this is quite concentrated, I've seen anything from 96% H2SO4 to as concentrated as 98% sulfuric as drain cleaner) This should be done afterwards to destroy the isocyanide, and thereby purge the offensive isonitrile miasma from whatever vessel the sample was tested in)
(As shown in this great online book)
http://www.books-about-california.com/Pages/Experimental_Organic_Chemistry/Ex_Organic_Chem_main.html
As for the chloroform synthesis itself, the reaction of a methyl ketone (or isopropanol as a specific case, also producing chloroform, presumably by oxidation of the hydroxyl group of iPA to a carbonyl by hypochlorite, giving acetone as an intermediate, which then undergoes the same reaction as acetone as a start point although of course consuming some NaOCl in the process) is called a haloform reaction, or haloform synthesis, and also works for bromoform (CHBr3 rather than CHCl3, chloroform) or the yellow solid compound iodoform (CHI3) although given the strong bonding between carbon and fluorine, the gaseous fluoroform, CHF3 must be produced if ever desired by alternative means. It works for the other halogens, fluorine excepted, although the weight yield, if done using hypochlorite (IIRC trichloroisocyanuric acid or sodium trichloroisocyanurate can be used for better yields) based upon acetone (the most expensive of the reagents used) is not fantastic, its serviceable. Especially if huge quantities of chloroform aren't needed. It is also quite exothermic, so either a mechanism to collect and condense the vapors given off will help recover more chloroform, a big haloform rxn generates an awful lot of heat, so condensing the vapors during the reaction will help, as will application of some cooling to the outside of the vessel the haloform reaction is performed in. (a big one can easily get so hot that you cannot touch the outside of the still without thick gloves, or a piece of asbestos mat, fiberglass cloth etc. to handle it)
For small quantities, its easy to make (insoluble in water btw, and like dichlor, its denser than water and if the two are together as with washing, brine washing to dry it by osmosis prior to a final distillation ideally, then the DCM or the chloroform layer is the bottom layer.) Chloroform has a distinctive sweetness to its 'solventy' smell, dichloromethane smells very similar but it lacks the sweetness shown by chloroform, its similar, but sharper but still with a hint of sweetness.
If you want to know what it smells like before trying to make some, then 'care+' brand codeine linctus actually uses chloroform as a preservative and it smells precisely like chloroform. Quite surprising really considering that CHCl3 is somewhat hepatotoxic. But, its in there, as preservative/flavouring (and that brand of codeine linctus has a very pleasant taste due to the chloroform in there, and its an essential ingredient in my 'manhattan project' cocktail-codeine linctus/lime soda/vodka/fresh lime juice and slices with a shot of diethyl ether trapped on top, diluted with 15-20ml or so good quality vodka or with sugared lime juice and 5ml or so of vodka. Hard to find that cough syrup these days OTC, but worth looking. Either on its own nice enough, but it makes a fantastic cocktail, invented that one myself. The codeine syrup flavoured with chloroform (no CHCl3 is added, its actually in there as manufactured) being heavy and dense and sugary, carefully layered on the bottom of a tall glass, and a fairly dilute (the ether has a real hefty kick) vodka solution in tesco own brand limeade with plenty of lime juice, a little honey or sugar to help balance the acidity of the lime juice layered over the top carefully, and finally something like a canal lock-gate constructed with three lime wedge, or two of lime and one of lemon (or vice versa if preferred) to trap a shot glass of ether at the top, close to the edge, consumed like a jagerbomb.
Chloroform, or dichloromethane (methylene chloride, CH2Cl2) are EXCELLENT solvents for purification of morphine, such as prior to acylation using acetic anhydride/acetyl chloride (or if one is to do such an esterification, its better to make the propionyl ester, because dipropionylmorphine has at least double the duration of action of heroin/morphine, and with less histamine release, its by my estimation about as potent again compared to heroin as heroin is to morphine, give or take a little either way, contrary to the wikipedia article on dipropionylmorphine it is faster, not slower acting than is heroin. And when injected packs a real whomper of a rush. If you've the choice then it simply isn't worth turning morphine to heroin when it can be made into dipropionylmorphine instead. It is, quite simply, superior in every single way it is possible to be so.
As for morphine itself, even purifying that so it can be taken nasally, or up the arse is better than no extraction.
Also, have read that even GAA (glacial acetic acid) can be used in place of acetic anhydride or acetyl chloride to acylate morphia, giving in that case, rather than diamorphine, 6-monoacetylmorphine. Would LOVE to try a pure 6-monopropionyl ester of morphine, only issue is that I'd have to go buy the glacial propionic acid, since my only other route to it would be hydrolysis of propionyl chloride which is a rather precious reagent in terms of the ease by which it may be obtained. GAA is easy off ebay. As are small quantities of acetic anhydride suitable for doing a few grams of morphine and making diamorphine.