- Preparation of Vinyl chloroacetate
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(CAS no ), which is also known as , chloro-, vinyl ester, could be produced through the following synthetic route.
A 1-l. three-necked flask is equipped with an efficient stirrer, a thermometer, a gas inlet tube 10 mm. in diameter, and a reflux condenser. The bulb of the thermometer and the lower end of the gas inlet tube are sufficiently close to the bottom of the flask to be covered by the reactants. The upper end of the condenser is attached to a small gas-washing bottle containing enough water so that the rate of passage of the exit gases may be noted. The flask is charged with 200 g. (2.12 moles) of monochloroacetic acid, 0.2 g. of hydroquinone, and 20 g. of yellow mercuric oxide. A slow stream of acetylene is passed through a spiral trap cooled in Dry Ice-acetone mixture, a mercury safety valve, an empty wash bottle, a sulfuric acid wash bottle, a soda-lime tower, and then into the reaction flask through the gas inlet tube. The stirrer is started, and the contents of the flask are heated gently with steam until the chloroacetic acid just melts. The temperature of the reaction mixture is lowered to 40–50° after 30 minutes or as soon as the melting point of the mixture permits the lower temperature to be attained without solidification. An ice bath is used for cooling the mixture when necessary. The stirrer is operated fast enough to throw the contents of the flask vigorously against the walls, in order to obtain the most rapid absorption. The absorption of acetylene, very rapid at first, becomes very slow after about 3 hours, and the introduction of the gas is discontinued.
The contents of the flask are decanted and filtered or centrifuged to remove as much as possible of the finely divided mercury salt. The filtrate is distilled from a Claisen flask, and 117–135 g. of material boiling at 45–55°/20 mm. is collected. The distillate is fractionated, and 107–125 g. (42–49%) of vinyl chloroacetate, b.p. 37–38°/16 mm., n25D 1.4422, is collected.
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