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	Posts 1 - 5 of 5	Subject: P2P / Chloroacetone



Jan1983 (Hive Bee) 06-24-02 03:01 No 324715	P2P / Chloroacetone	Bookmark Reply
	Swij is at a very good mood toaday and looked around the p2p synth's now he's going into the Chloroacetone synth. As normal Swij isnt that good chemist, so here are some questions before starting. Original: Good method of preperation 150 ml acetone 50 ml water 12 g Cupric chloride 6 g lithium chloride. Reflux till reaction completes. Literature states 24 hours but the reaction has a half-life of about 24 minutes at 20°C (same article half of marker in 24 minutes, the marker being oxygen consumption in a slightly different reaction), therefore 5 hours is probably sufficient at reflux. Swim got 500ml 99,98% pure (for GC) stuff from Merck so he wanted to start 500ml acetone + 166ml water + 60g cupric chloride(CuCl2) no LiCL2 avail at the moment 1.) is the calculation correct ? 2.) does it need to be destilled twice ? Chloroacetone must be stabalized with 1% calcium carbonate or 0.1% water if it is stored 3.) can i use Potassium / Sodium carbonate instead of calcium carbonate too ? 41 grams (0.31 mole) of anhydrous aluminum chloride and 100 ml of anhydrous benzene (free from thiophene) were put in a 500ml three-necked flask which was equipped with a mercury-sealed stirrer, a reflux water condenser and a small addition funnel. The top of the condenser was connected to a sulfuric acid trap and this trap was connected to a gas absorption bottle. The mixture was stirred and heated to refluxing on a steam bath and 13.9 g (0.15 mole) of chloroacetone was allowed drop in slowly during a period of 30 minutes. After refluxing for 5 hours, the solution was practically black. After cooling to room temperature, the reaction mixture was decomposed by slowly adding water through the condenser, stirring during the addition. When no more hydrogen chloride was evolved, 20 ml of water and 20 ml of concentrated hydrochloric acid was added. The benzene layer was separated and the aqueous layer extracted with four 25 ml portions of benzene. All of the benzene solutions were combined and filtered. The benzene was distilled off, and the remaining viscous oil was distilled under reduced pressure. Nine grams of liquid boiling below 123°C/20-22mmHg was obtained. Approximately 10g of high-boiling material was left in the distilling flask. Phenyl-2-Propanone was recovered from the distillate by making the bisulfite addition product, filtering, decomposing the addition product with sodium carbonate solution, and steam distilled as long as any oil distilled over. The distillate was extracted with ether, the ether dried over anhydrous MgSO4 and the ether distilled on a steam bath. The phenyl-2-Propanone was distilled under reduced pressure, bp 108-114°C/20-22mmHg. Yield 6.5 g (32%). 4.) Cant the 100ml benzene used at first, be exchanged with another nonpolar solvent like toluol ? 5.) Can a magnetic stirrer also be used ? Chemistry are not only the things that stink. :)



Elementary (Hive Addict) 06-24-02 03:18 No 324721	Umm	Bookmark Reply
	can i use Potassium / Sodium carbonate instead of calcium carbonate too ? Are you trying to tell us that you can't find chalk OTC ? John Lennon - Working Class Hero



lugh (Moderator) 06-24-02 04:42 No 324739	Tear Gas	Bookmark Reply
	Cant the 100ml benzene used at first, be exchanged with another nonpolar solvent like toluol? No, unless you're seeking methylphenyl2propanone You need to study Friedel-Krafts reactions much more thoroughly before going any further Can a magnetic stirrer also be used? Tar formation makes magnetic stirring useless The Friedel-Krafts reaction can proceed without stirring, albeit with lower yields Chloroacetone has been used as tear gas, you'll find these syntheses to be quite noxious, and low in yield as well Unless you have a suitable fume hood, forget about it



foxy2 (Distinctive Doe) 06-24-02 12:29 No 324831	while your at it	Bookmark Reply
	maybe look into bromoacetone, its a little less volitile but still extremely noxious Those who give up essential liberties for temporary safety deserve neither liberty nor safety



former_chemist (Hive Bee) 06-24-02 22:34 No 325055	Wrong calcs	Bookmark Reply
	1) Ok no your calculations are wrong. 500/150=3.33 3.33*12 = 40 not 60 Lack of LiCl means the reaction will be much slower. React lithium carbonate (readily available) with HCl and Evaporate. 2) Distilling twice is not absolutely necessary but is highly recommended. Excess water and/or acetone and/or dichloroacetone will ruin its usability as a reactant. 3) Somewhere on the internet is a good production method for chalk from calcium chloride and sodium carbonate. Otherwise buy white carpenters chalk. It contains titanium oxide as an impurity. DON'T use sodium carbonate, it causes some unwanted reactions. 4) Benzene is a reactant not a solvent. It cannot be substituted. 5) A mechanical stirrer is recommended because a magnetic doesn't have the torque. Stronger stirrers might work with an oversized stir bar. Unasked questions are the most telling. The first reaction is pretty fool proof if a bit smelly and not particularly high yielding. The cleanup is the bad part. The yeild from 40g of CuCl2 is only 6 grams or so. The final step is making the product anhydrous, be careful how that is handled. The second reaction requires ANHYDROUS conditions. Using water as the stabilizer will ruin the second reaction. Also the Aluminum Chloride MUST be ANHYDROUS. An interesting use of the off gas of a friedel-crafts is converting amines to HCl salts or poisoning your neighbors.

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