The synthetic route of 624-95-3 has been constantly updated, and we look forward to future research findings.
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.
EXAMPLE III; Example III illustrates the oxidation of 3, 3-dimethyl-1-butanol to 3, 3-dimethyl-1- butanal using the catalyst system of the current invention: 170 mg ofFe (N03) 3′ 9H20 (0.416mmol), 66mg 2,2′-bipyridyl (0.416mmol), 85mg TEMPO (0.536mmol) and 80mg N-bromosuccinimide (0.45mmol) are dissolved in glacial acetic acid (7 cc) and the solution transferred into a jacketed glass reactor. The reactor is alternately evacuated and purged with oxygen at least five times and the temperature of the catalyst solution is raised to the target value of 45C under constant stirring of 1500RPM. When the temperature reached 45C, 8200 mg of 3, 3-dimethyl-1- butanol (76. 6mmol) are injected through the septum adapter using a gas tight syringe. The recorded oxygen uptake rate is 0. 205mmol 02/min and the GC analysis after 250min reaction time showed 95.2% conversion of the starting alcohol and 96.2% selectivity to the desired 3, 3-dimethyl-l-butanal. The graphical presentation of this reaction is also shown in the same Figure 01, curve 3, NS 10 16.EXAMPLE IV Example TV represents the potential of the catalyst composition to be used at even higher alcohol concentration in direct comparison with Example III. 170 mg of Fe (N03) 3 9H20 (0. 416mmol), 66mg 2,2′-bipyridyl (0. 416mmol), 85mg TEMPO (0. 536mmol) and 80mg N-bromosuccinimide (0. 45mmol) are dissolved in glacial acetic acid (7 cc) and the solution transferred into a jacketed glass reactor. The dissolution and thermostating of the catalyst solution is done as in Example III. When the temperature reached 45C, 9840 mg of3, 3-dimethyl-l-butanol (91. 9mmol) are injected through the septum adapter using a gas tight syringe. The recorded oxygen uptake rate was 0. 184mmol 02/min and the GC analysis after 420min reaction time showed 89.2% conversion of the starting alcohol and 97.4% selectivity to the desired 3, 3-dimethyl-1- butanal. The graphical presentation of this reaction is also shown in the same Figure 01, curve 4, NS1027. EXAMPLE V Example V represents addition protocol in which the catalysts solution and the alcohol are charged in the reactor prior purging the reactor with oxygen and raising the temperature. 170 mg ofFe (N03) 3′ 9H20 (0. 416mmol), 66mg 2, 2′-bipyridyl (0. (d416mmol), 85mg TEMPO (0. 536mmol), 80mg N-bromosuccinimide (0. 45mmol) and 8200 mg of 3, 3-Dimethyl-l-butanol (76. 6mmol) are dissolved in glacial acetic acid (7 cc) and the solution transferred into a jacketed glass reactor. The dissolution and therniostating of the catalyst solution is done as in Example III. When the temperature reached 45C the stirring rate was set to 1500RPM and at this point, monitoring of the oxygen uptake was initiated. The recorded oxygen uptake rate was 0. 220rrunol 02/min and the GC analysis after 230min reaction time showed 96.3% conversion of the starting alcohol and 98.5% selectivity to the desired 3, 3-dimethyl-1-butanal. The graphical presentation of this reaction is also shown in the same Figure 01, curve 5, NS1019.
The synthetic route of 624-95-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; THE NUTRASWEET COMPANY; WO2005/82825; (2005); A1;,
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Alcohols – Chemistry LibreTexts