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 Production Method of Methyl benzyl ketone
  • Production Method of Methyl benzyl ketone
  • Methyl benzyl ketone (CAS NO.: ), which is also known as 1-phenyl-2-propanone, could be produced through the following synthetic route.

    Production Method of Methyl benzyl ketone

    The reaction is carried out in the apparatus shown in Fig. 13. A-A is a Pyrex combustion tube, 90 cm. long and 2 cm. in diameter, fitted with an inlet chamber B, having a sealed-in side arm C and bearing a separatory funnel E. The center 60 cm. of the tube is filled with thorium oxide catalyst held in place at the lower end by indentations in the combustion tube. The hot junction D of a pyrometer is placed in contact with the glass tube at its center, and the catalyst-filled section of the tube is wrapped with a thin layer of asbestos paper. The tube is supported in an electrically heated cylindrical furnace, 60 cm. in length, which is inclined slightly from the horizontal. The annular space between the tube and the furnace is plugged at the ends with asbestos in order to produce a uniform temperature throughout the tube and to hold the glass tube in place. The lower end of the reaction tube is connected through the adapter F to a vertical glass tube G, 40 cm. long and 2 cm. in diameter, which is filled with glass beads and serves as the condenser. An Erlenmeyer flask or other suitable receiver is placed at the lower end of G.

                                                 Fig. 13

    Fig. 13

    The furnace is heated to 430–450°, and simultaneously the tube is swept out thoroughly with a stream of carbon dioxide, introduced through the side arm C. The carbon dioxide is passed through a wash bottle of concentrated sulfuric acid to dry it and to estimate the rate of flow. A solution of 136 g. (1 mole) of phenylacetic acid, m.p. 77–79°, in 120 cc. (120 g., 2 moles) of glacial acetic acid is placed in the separatory funnel E and is introduced into the inlet chamber B at the rate of twelve to fifteen drops per minute. The entire solution should run through in twelve to fifteen hours. Meanwhile a very slow stream of carbon dioxide (one bubble per second) is passed through the tube C, to keep the gases in motion. After all the solution has been added, the funnel is rinsed with 10 cc. of glacial acetic acid, and this is passed through the reaction tube to facilitate removal of the product. The distillate consists of a slightly fluorescent light brown oil and an aqueous layer; both layers are treated with 300 g. of a mixture of ice and water, and rendered alkaline to litmus with a slight excess of 50 per cent sodium hydroxide solution.

    The oil is separated, and the aqueous layer is extracted with two 50-cc. portions of benzene. The extracts are combined with the oil, and the solvent is removed by distillation. Fractionation of the residue under reduced pressure gives 80–95 g. of a methyl benzyl ketone fraction, boiling at 110–120°/21–22 mm., and a residue of dibenzyl ketone. The main fraction on redistillation yields 74–87 g. (55–65 per cent of the theoretical amount) of methyl benzyl ketone boiling at 110–115°/21–22 mm.


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