Synth: Chloroform from Calcium Hypochlorite and Ethanol

The Watcher · Dream Team

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DICHLORMETHYL CHLORIDE ( CHLOROFORM (U.S.Ph)), (CHCL4,Cl)

Mw. 120.5

It is obtained by heating in a large still 35 to 40 liters H2O, adding 10 Kilos Calcium Hypochlorite, add 2.5 kilos ethyl alcohol, then the raise the temperature quickly until the product begins to distil, turn off the heat, then apply the heat again at the end of the reaction. The crude chloroform so obtained is purified by first shaking it with H2SO4, then by mixing with alcohol and potassium carbonate and distilling the mixture.

It is a colorless, volatile liquid, having a strong agreeable, ethereal odor, and a sweet taste.

Sp.Gr. 1.497

Sparingly soluble with H2O, miscible with alcohol and either in all parts.

Bp 60.8 Deg.C.

It is a good solvent for many substances insoluble in H2O, such as phosphorus, iodine, fats, resins, caouutchouc, gutta-percha and alkaloids.

CHLOROFORM (CHCl3)

(This is taken from THE WATCHERS lab notebook).

Properties of Product and Compounds.

Chloroform (CHCl3) - Bp. 61 deg.C.... Sp.Gr. - 1.492

Calcium Hypochlorite (CaCOCl)2 - Mp. 100 Deg.C....SpGr. 2.350

Ethyl Alcohol (C2H5OH) - Bp. 78 Deg.C. SpGr. .794

Water (H2O) - Bp. 100 Deg.C....SpGr. - 1

In a 100 Ml distilling flask place 50 Ml H2O, 6 Ml Alcohol, and 10 Gr Calcium Hypochlorite, assemble distillery and apply heat.

When the temperature reached 24.5 Deg.C. the reaction mixture turned a milky white and there was some condensation in the distilling head. The first drop came over at 40 Deg.C. When the temperature stabilized at 80 Deg.C. two small layers came over in the receiver adjusted the temperature till it was at 76 Deg.C. continued to distill.

When the temperature dropped rapidly the reaction was finished.

When the receiver was moved the two layers combined

Added 2.5 mL H2O and .5 mL H2SO4 shake and separate the layers.

There was .5 Ml Chloroform left.

Note: did the same experiment as above only mixed 2.5 mL ethyl alcohol with .5 mL H2SO4 and distilled the mixture then shook the final product of this distillation with .5 mL H2O and sodium bicarbonate and was left with .9 mL chloroform.