- Preparation of β-Methyl-δ-valerolactone
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β-Methyl-δ-valerolactone (CAS no.: ), which is also called as , 5-hydroxy-3-methyl-, δ-lactone, could be produced through the following synthetic route.
A 1-l. three-necked flask fitted with an efficient stirrer, a thermometer, and a reflux condenser attached to a device for measuring gas evolution is charged with 197 g. (1.67 moles) of 3-methyl-1,5-pentanediol and 10 g. of copper chromite. The mixture is heated rapidly to 200° with good stirring and is held at 195–205° for 1.5–3.0 hours, during which time 3.1 cu. ft. of hydrogen is evolved. The product is distilled directly from the flask with stirring through a 2 by 120 cm. Vigreux column. The yield of β-methyl-δ-valerolactone is 172–180 g. (90–95%), b.p. 110–111°/15 mm., nD25 1.4495.
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