Application of 59997-51-2, A common heterocyclic compound, 59997-51-2, name is 4,4-Dimethyl-3-oxopentanenitrile, molecular formula is C7H11NO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
128 mL of water was added to 50 g (357 mmol) of the intermediate (c), and the mixture was stirred at room temperature, 98.2 g (785 mmol) of pivaloyl acetonitrile was added to this suspension, 12M hydrochloric acid water was added dropwise at the same temperature so that the pH became 3, The mixture was heated to an internal temperature of 50 C. and stirred at the same temperature for 6 hours. After completion of the reaction, 8N aqueous solution of calcium hydroxide was added to neutralize the solution to pH 6.4. The crystals thus precipitated were collected by filtration and washed with water until the inner temperature became 10 C. The obtained crystals were dried under reduced pressure at 60 C. and 30 mL of toluene was added to the obtained crude product In addition, it was dissolved by heating to 60 C. The resulting solution was allowed to stand at room temperature for 12 hours, and the precipitated crystals were collected by filtration, washed with cold toluene, dried at 60 C. under reduced pressure,The obtained intermediate (d) was obtained in 87.7 g (white powder, yield 69.3%), and the NMR measurement results of the obtained intermediate (d) are as follows.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; FUJIFILM Corporation; Tateishi, Keiichi; Sasaki, Hiroki; Nagata, Yoshiaki; (37 pag.)JP2017/61660; (2017); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts