Synthetic Route of 624-95-3 , The common heterocyclic compound, 624-95-3, name is 3,3-Dimethylbutan-1-ol, molecular formula is C6H14O, 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.
16.9 g of 3, 3-Dimethyl-l-butanol (117.3 mmol) and 0.0765 g MeO-TEMPO (0. 411MMOL) are charged in a jacketed glass reaction flask as in Example I. Sodium borate (0.380 g, 1.0 mmol) and potassium bromide (0.011 g, 0.104 mmol) are dissolved in water (12.0 cc) and the aqueous solution is added to the stirred organic fraction at 1000 RPM in the reaction flask. The stirred suspension is cooled to 0C and the emulsion is re- adjusted to pH 8.4 using 50% solution of CH3COOH. When the temperature of the reactants reached 0C, 75.5 g (122 mmol) of 12. 1% aqueous NAOCI solution are pumped in via a gas-tight syringe over 90 minutes (The pH of the bleach solution was adjusted to 10 using 50% aqueous CH3COOH). During the bleach addition the pH was maintained at 8.3-8. 4 levels using a few drops of 50% aqueous CH3COOH. The reaction mixture is stirred for an additional 120 min at 0C and the organic layer is sampled for GC assay. The reaction in this second stage was kept at pH 8.4 by addition of 0.2-0. 25 cc aqueous solution OF NAOH (50% concentration). The yield of 3, 3-dimethylbutyraldehyde is 94.0% at 60 min and 95.0% at 90 min reaction time. This yield is equivalent to the yield of Example III in which no potassium bromide was used.
The synthetic route of 624-95-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; THE NUTRASWEET COMPANY; WO2004/67484; (2004); A2;,
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