posted March 11, 2000 04:06 PM            

Nitromethane
[1]Dissolve 50g of mono-chloroacetic acid in 100 ml water contained in a 500 ml round-bottomed bolt-head flask, and then neutralise the solution by the cautious addition of 30g of finely powdered anhydrous sodium carbonate. For this purpose, add the sodium carbonate in small quantities (about 1g) at a time, preferably with the aid of a spatula, and shake the solution gently around after each addition to facilitate the evolution of carbon dioxide: a clear solution is thus maintained throughout, whereas the rapid addition of large quantities of the carbonate produces lumps of material which are subsequently difficult to dissolve. Now dissolve 36.5g of sodium nitrite in 50 ml of water with gentle heating, cool the solution thoroughly in icewater, and then add it with shaking to that of the sodium monochloroacetate. Add some fragments of unglazed porcelain, and then fit the flask with a delivery-tube of moderately wide bore connected in turn to a water-condenser. Support the flask over a gauze, and then heat it gently with a small Bunsen flame. The solution slowly becomes yellow in colour, then greenish and finally a yellowish-brown, when a vigorous effervescence starts: at once remove the Bunsen flame, and allow the reaction to proceed spontaneously, carbon dioxide being evolved and the solution boiling vigorously. When the reaction subsides, replace the Bunsen flame and maintain a steady boiling. Nitromethane distills over in the steam and separates as a colourless oil at the bottom of the distillate: since nitromethane is slightly soluble in water, stop the distillation as soon as drops of nitromethane can no longer be detected in the distillate leaving the condenser. Transfer the distillate to a separating- funnel, and carefully run off the lower layer of nitromethane and then dry it over anhydrous sodium sulfate for 30 minutes. Filter the dry nitromethane (preferably through a small dry Buchner funnel), transfer it to a 30 ml. distilling-flask fitted with a water-condenser, and then slowly distill, collecting the fraction of bp 100-102°C. In view of the small volume of nitromethane to be manipulated, if a small Buchner funnel is not available, it is advisable to extract the crude nitromethane from the aqueous distillate with ether (30-40ml). Dry the ethereal extract over sodium sulfate, filter through a fluted filter-paper, and then distill off the ether on a water-bath, and finally distill the residual nitromethane. Nitromethane is obtained as a colourless liquid, of bp 101°C and d 1.10, yield, 10 g.

acetic acid
1. Buy the strong 9% vinegar for making pickles. Choose the clear kind, not the Red Wine or other flavored varieties. 2. Neutralize with lye. Just add lye until no more bubbling/fizzing. This will leave you with an aqueous solution of Sodium Acetate. 3. Evaporate the solution to recover solid sodium acetate salt. 4. Make a solution of dilute H2SO4. 5. Mix the acid with the sodium acetate. This will give you a solution of Sodium Sulfate and acetic acid. 6. Distill to collect the acetic acid. The azeotrope comes at 107C and pure comes over at 118. Collect between 105 and 120 or dryness (whichever comes first) 7. If you need it to be relatively free of water (near glatial) then dry it and redistill collecting between 115ish and 120.

Notice( number 4: It say use dilute, dont know why, id rather use consentrated.

-->Yes! it's possible!

Chloroacetic acid or monochloroacetic acid
(ClH2C-COOH) colorless to light-brownish, corrosive, crystals. which is very soluble in water and other organic solvents. Melting point (3 modifications): 63 C, 56 C, 53 C.
Boiling point: 188 C. Prep.:

-through chlorination of glacial
acetic acid in the presence of
catalytic amounts of sulfuric acid
or iodine.

-by action of chlorine on acetic acid
in the presence of acetic anhydride, phosphorus, or sulfur.

posted March 12, 2000 03:52 AM            

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Dry chlorine is led into a mixture of 150 g. of glacial acetic acid
and 12 g. of red phosphorus contained in a flask (Fig. 47, p. 104), which
is provided with a delivery tube and a reflux condenser and is heated
on a vigorously boiling water bath. The flask should stand in a
well-lit place, preferably in direct sunlight, since the rate of chlorination
greatly depends on the illumination. As soon as a small portion
of the mixture solidifies when cooled with ice-water and rubbed
with a glass rod, the reaction is complete. In summer one day
suffices, but on dull winter days the passing in of chlorine must be
continued for a second day. To isolate the monochloroacetic acid
the product of the reaction is fractionally distilled from a flask fitted
with an air condenser; the fraction which passes over at 150”-200”
is separately collected in a beaker. The beaker is cooled with ice-water
while its contents are stirred with a glass rod and the portion
which solidifies, consisting of pure monochloroacetic acid, is rapidly
filtered at the pump; the loose crystals are firmly compressed with
a spatula or pestle. The filtration must not be continued too long
or the chloroacetic acid will gradually be liquefied by the heat of the
air. The filtrate is redistilled, the portion passing over between
170” and 200” being separately collected. By repetition of the
process just described (cooling and filtering) a second portion of
monochloroacetic acid is obtained. It is combined with the main
portion and the whole is completely purified by a further distillation;
b.p. 186”, m.p. 63", yield, variable : 80-125 g. Used for the prepara-tion
of nitromethane (p. 156), diethyl malonate (p. 254), glycine (p. 275),
phenylglycine (p. 369).
Since monochloroacetic acid, especially when warm, attacks the
skin severely, care is indicated.
The chlorination proceeds considerably more rapidly, and also in
the absence of light, if 1.5 g. of iodine, 7 g. of phosphorus pentachloride,
and 3 g. of red phosphorus are added to the 150 g. of glacial acetic acid
mentioned above.2 When the reaction is over, the hot mixture is de-canted
from the phosphorus, diluted with 40 c .c of glacial acetic acid,
and cooled. The monochloroacetic acid which crystaliises is rapidly
filtered and washed with a little glacial acetic acid. In this way a
pale red product results, which is freed from adherent iodine by stand-ing
in a desiccator over potassium hydroxide.
1 R. Hoffmann, annalen, 1857, 102, 1; Russanow, Ber., 1892, 25, Rd. 334.
2 H. Briickner, Z. angew. Chem., 1927,40, 973; 1928, 41, 226.