- Preparation of Chloroacetonitrile
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Chloro (CAS NO.: ), which is also known as Acetonitrile, chloro-, could be produced through the following synthetic route.
In a 3-l. round-bottomed three-necked flask fitted with an efficient mechanical stirrer, a reflux condenser, and a thermometer are placed 170 g. (1.2 moles) of phosphorus pentoxide, 187 g. (2 moles) of chloroacetamide2, and 800 ml. of dry technical trimethylbenzene. The mixture is refluxed gently with vigorous stirring for 1 hour. The reaction mixture is then allowed to cool to about 100° with continuous stirring, and the reflux condenser is replaced with a distilling adapter fitted with a thermometer and a water-cooled condenser.
The crude product and part of the solvent are distilled at atmospheric pressure. The yield of crude product boiling at 124–128° is 121–131 g. (80–87%) (nD25 1.441–1.444). In order to obtain a pure product, the crude is mixed with 10 g. of phosphorus pentoxide and redistilled through an efficient packed fractionating column. The yield of pure chloroacetonitrile distilling at 123–124° is 93–106 g. (62–70%).
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