Trap for absorbing gases

A 1-1. three-necked round-bottomed flask is mounted on a steam cone and is fitted with a 250-cc. separatory funnel and a reflux condenser connected to a trap (Note 1) for absorbing gases. In the flask is placed 325 g. (198 cc., 2.73 moles) of thionyl chloride (Note 2), and to it is added, during the course of one hour, 125 g. (0.58 moles) of /-menthoxyacetic acid (p. 52). The flask is shaken frequently during the addition of the acid and, if necessary, is warmed to start the reaction. When all the acid has been added... 

Blind column connections and maintain good ventillation during hot work. Watch out for absorption of gases in wash water. The absorbed gases can be released at undesirable locations. These gases can be trapped in the system even after the wash. 

A 101.3-mg sample of an organic compound known to contain Cl is burned in pure O2 and the combustion gases collected in absorbent tubes. The tube used to trap CO2 increases in mass by 167.6 mg, and the tube for trapping H2O shows a 13.7-mg increase. A second sample of 121.8 mg is treated with concentrated HNO3 producing CI2, which subsequently reacts with Ag+, forming 262.7 mg of AgCl. Determine the compound s composition, as well as its empirical formula. 

B. a-Hydroxyphenazine (demethylalion). A solution of 4.2 g. (0.02 mole) of a-methoxyphenazine, from A above, in 125 ml. of 55% hydrobromic acid (Note 7) is placed in a 250-ml. round-bottomed flask fitted with a reflux condenser. The flask is immersed in an oil bath, and the solution is heated to 110-120° for 5 hours the evolved gases are absorbed with water in a trap. The reaction mixture is cooled to room temperature, diluted with about 125 ml. of water, almost neutralized with sodium hydro.xide (Note 8), and extracted six times with 30- to 40-ml. portions of ether. The combined ether extracts arc extracted with 25-ml. portions of 10% sodium hydroxide solution (Note 9) until no more purple sodium salt is remox ed from the ether. The aqueous extracts are combined, made acid to litmus with dilute acetic acid, and re-extracted four times with 50-ml. portions of ether. The combined ether extracts are dried over anhydrous sodium sulfate, and the ether is removed by distillation on a steam bath. The residue is recrystallized as follows It is dissolved in the least possible amount of hot alcohol, water... 

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