- Preparation of Ethyl benzoylacetate
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(CAS NO.: ), which is known as , benzoyl-, ethyl ester, could be produced through the following synthetic routes.
In an open 3-l. three-necked flask, equipped with an efficient mechanical stirrer and two dropping funnels, are placed 500 ml. of water, 250 ml. of technical naphtha boiling at 95–110°, and 195 g. (1.5 moles) of freshly distilled ethyl acetoacetate. The mixture is cooled to 5° with a water-ice bath, and 65 ml. of 33% sodium hydroxide solution (33 g. sodium hydroxide in 100 g. solution) is added. As the temperature is maintained below 10°and the pH near 11, the mixture is stirred vigorously, and there are added simultaneously from the two dropping funnels 230 g. (1.62 moles) of benzoyl chloride and 270 ml. of 33% sodium hydroxide solution. This addition should be made during about 2 hours. After addition is complete, the cooling bath is removed, and the mixture is allowed to come to room temperature. In order to ensure complete reaction, the mixture is finally brought to 35° during about 1 hour. The stirrer is then stopped, and the aqueous layer is separated and placed in a 2-l. Erlenmeyer flask.
To the mixture is added 80 g. of technical ammonium chloride; then it is stirred slowly overnight. The specific gravity is brought to 1.13 by the addition of about 90 g. of sodium chloride, after which the mixture is transferred to a separatory funnel. About 10 ml. of benzene is used to rinse the flask and is added to the separatory funnel. The aqueous layer is withdrawn, and the oil is washed three times with 100-ml. portions of cold water.
An additional 40 ml. of benzene is added (to accomplish drying on distillation), and the product is distilled under reduced pressure, using a short still head with no fractionating column. The yield of ethyl benzoylacetate, b.p. 145–150°/12 mm., is 197–203 g. (68–71%).
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