Electric Literature of 6624-71-1,Some common heterocyclic compound, 6624-71-1, name is Dodecyl isobutyrate, molecular formula is C16H32O2, 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.
EXAMPLE I Dodecyl 3-hydroxy-2,2,3-trimethyl-4-oxopentanoate STR7 To a solution of diisopropylamine (5.56 g, 0.055 mole) in 200 ml of dry ether at 0 C. under nitrogen is added with stirring n-butyllithium (0.055 mole) in hexane (31 ml). The resulting mixture is cooled to -70 C., and a solution of dodecyl isobutyrate (12.8 g, 0.05 mole) in ether (25 ml) is added dropwise over a period of 20 minutes. The mixture is warmed to -15 C., and a solution of 2,3-butanedione (4.73 g, 0.055 mole) in ether (10 ml) is added rapidly. The mixture then is stirred at -5 C. for 15 minutes. The reaction mixture is combined with 200 ml of saturated ammonium chloride solution, and the separated organic layer is washed in sequence with 200 ml of 0.5N HCl, 200 ml of saturated sodium bicarbonate, and 200 ml of saturated sodium chloride. The solution is dried over magnesium sulfate and the solvent is removed under reduced pressure to give 19 g of an oil. The oil is distilled in a Kugelrohr apparatus (air bath temperature 85-115 C. at 0.1 mm Hg) to provide 13.5 g of almost pure product. Fractional distillation of the oil yields 11.5 g of pure product (67%), b.p. 132-133 C. at 0.05 mm Hg. IR and NMR data confirm the above structure. Anal. calc. for C20 H38 O4: C, 70.13; H, 11.18. Found: C, 70.11; H, 11.24.
The synthetic route of 6624-71-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Philip Morris Incorporated; US4701282; (1987); A;,
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