|Manufacture of organic acid chlorides||Bookmark|
From Patent GB401643
The processes described here use phosgene which is very poisonous gas. You should be very careful when dealing with such chemicals and you should use proper protection equipment, such as gloves and gas mask. The reactions should be performed in the fume hood or in the well ventilated area.
Read MSDS for Phosgene http://www.boc.com/gases/pdf/msds/G067.p
Example 18: Oxalyl chloride
9 parts of anhydrous oxalic acid in 15 parts of diethyl aniline are dissolved in 70 parts nitrobenzene whilst heating. When cold the solution is run into a solution of 20 parts of phosgene in 25 parts of nitrobenzene whilst cooling. The whole is stirred for some time at ordinary temp and the oxalyl chloride which is formed is recovered by fractional distillation.
The production of oxalyl chloride can also be conducted in the abscence of a solvent.
Example 29: Oxalyl chloride
12.5 parts of ammonium oxalate are suspended in 40 parts of anhydrous formic acid and 20 parts of phosgene are introduced gradually whilst cooling with ice and stirring. The whole is stirred further for some time at room temp and the oxalyl chloride is isolated directly by fractional distillation.
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