Category: 624-95-3

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;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 624-95-3, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 624-95-3, name is 3,3-Dimethylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

12. 2’G OF 3, 3-DIMETHYL-1-BUTANOL of 98% purity (117. 3 mmol) and 0.043 g MEO- TEMPO (0. 223MMOL) are charged in a jacketed glass reaction flask as in Example I. Sodium borate (0.294 g, 0.76 mmol), NAHCO3 (1.472 g, 17.5 mmol) and NaCl (2 g) are dissolved in water (25 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 8.6 using 40% solution OFNAOH. When the temperature of the reactants reached 0C, 69.8 g (123.1 mmol) of 13.1% aqueous NAOCI solution are pumped in via a gas-tight syringe over 55 minutes. The reaction mixture is stirred for an additional 15 min at 0C and the organic layer is sampled for GC assay. The yield of 3,3- dimethylbutyraldehyde is 90.6% at 2 min of post bleach-addition time and 92. 1% at 15 min reaction time.

According to the analysis of related databases, 624-95-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; THE NUTRASWEET COMPANY; WO2004/67484; (2004); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Electric Literature of 624-95-3 ,Some common heterocyclic compound, 624-95-3, 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.

Dimethylsulfoxide (6.80 mL, 95.7 mmol) was added over 5 min to a solution of oxalylchloride (23.9 mL, 47.8 mmol) in dichloromethane at -78 0C. The resulting mixture was stirred at -78 0C for 5 min, then 3,3-dimethyl-butan-l-ol (5.22 mL, 43.1 mmol) was added. After stirring an additional 30 min at -78 0C, triethylamine (23.3 mL, 167 mmol) was added and the reaction mixture warmed to 0 0C and stirred at that temperature for 45 min. The mixture was then transferred to a separatory funnel and was washed with 0.5 M aqueous hydrochloric acid. The organic layer was dried over sodium sulfate, filtered and was concentrated in vacuo to a volume of about 70 mL (water bath temperature = 0 0C). Methanol (100 mL) was added followed sequentially by 1 -amino- lH-pyrrole-2-carboxylic acid allyl ester (Example Ib, 7.16 g, 43.1 mmol), acetic acid (6 mL), and sodium cyanoborohydride (5.42 g, 86.3 mmol). The reaction mixture was stirred at 23 0C for 2 h, and then was partitioned between saturated aqueous sodium bicarbonate solution (400 mL) and a 1 : 1 mixture of ethyl acetate and hexanes (2 x 200 mL). The organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. Purification of the residue by flash column chromatography (Merck silica gel 60, 40-63 mum, 5?10% ethyl acetate in hexanes) afforded the desired product, l-(3,3-dimethyl-butylamino)-lH-pyrrole-2- carboxylic acid allyl ester (4.04 g, 16.15 mmol, 37% yield) as a clear liquid. 1H NMR (400 MHz, CDCl3) delta: 0.91 (9H, s), 1.42 – 1.46 (2H, m), 2.98 – 3.04 (2H, m), 4.75 – 4.77 (2H, m), 5.26 – 5.28 (IH, m), 5.37 – 5.41 (IH, m), 5.96 – 5.99 (IH, m), 6.01 – 6.05 (IH, m), 6.27 – 6.30 (IH, m), 6.89 – 6.91 (IH, m), 6.96 – 6.98 (IH, m).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,624-95-3, its application will become more common.

Reference:
Patent; ANADYS PHARMACEUTICALS, INC.; WO2007/150001; (2007); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 624-95-3, name is 3,3-Dimethylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. 624-95-3

Example IV represents an oxidation in which the KBr co-catalyst and the NaHCO3 buffer were removed and replaced with Na2B4O7 additive. [00065] 16.9 g of 3,3-Dimethyl-1-butanol (117.3 mmol) and 0.0765 g MeO-TEMPO (0.411 mmol) are charged in a jacketed glass reaction flask as in Example I. Sodium borate (0.380 g, 1.0 mmol) is 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 0 C. and the emulsion is re-adjusted to pH=8.4 using 50% solution of CH3COOH. When the temperature of the reactants reached 0 C., 75.5 g (122 mmol) of 12.1% aqueous NaOCl solution are pumped in via a gas-tight syringe over 90 minutes. 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 0 C. 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 90.0% at 60 min and 91.0% at 90 min reaction time

Statistics shows that 624-95-3 is playing an increasingly important role. we look forward to future research findings about 3,3-Dimethylbutan-1-ol.

Reference:
Patent; The NutraSweet Company; US6825384; (2004); B1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 624-95-3 as follows., 624-95-3

2.24 g (51.3 mmol) of 55 wt% sodium hydride was suspended in 100 ml of tetrahydrofuran. 4.24 g (41.5 mmol) of 3,3-dimethylbutanol was added dropwise to the suspension under ice cooling, and the mixture was stirred at room temperature for 15 minutes. To this was added dropwise 20 ml of a tetrahydrofuran solution of 5.0 g (37.7 mmol) of 2-chloro-5-fluoropyrimidine, followed by stirring at room temperature overnight. A saturated aqueous solution of ammonium chloride was added thereto, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the inorganic matter was removed by filtration. The filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 4.40 g (22.2 mmol, yield 59%) of 2- (3,3-dimethylbutoxy) -5-fluoropyrimidine.

The chemical industry reduces the impact on the environment during synthesis 624-95-3, I believe this compound will play a more active role in future production and life.

Reference:
Patent; NIPPON SODA COMPANY LIMITED; ITO, SYUICHI; AMANO, TOMOHIRO; IPPOSHI, JUNJI; KOUBORI, SHINYA; (44 pag.)JP2016/30742; (2016); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 624-95-3, name is 3,3-Dimethylbutan-1-ol, the common compound, a new synthetic route is introduced below. 624-95-3

12.2 g of 3, 3-Dimethyl-l-butanol of 98% purity (117.3 mmol) and 0.036 g TEMPO (0.223mmol) are charged in a jacketed glass reaction flask as in Example I. Sodium borate (0.294 g, 0.76 mmol), NAHCO3 (1.472 g, 17. 5MMOL) and NACL (2 g) are dissolved in water (25 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 8.6 using 40% solution OF NAOH. When the temperature of the reactants reached 0C, 69.8 g (123.1 mmol) of 13.1% aqueous NAOCI solution are pumped in via a gas-tight syringe over 55 minutes. The reaction mixture is stirred for an additional 15 min at 0C and the organic layer is sampled for GC assay. The yield of 3,3- dimethylbutyraldehyde is 87.4% at 2 min of post bleach-addition time and 91.2% at 15 min reaction time.

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;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

624-95-3, A common compound: 624-95-3, name is 3,3-Dimethylbutan-1-ol,molecular formula is C6H14O, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

[00072] Example VIII is similar to VII but the amount of MeO-TEMPO is reduced twice. All other concentrations and ratios are the same as in Example VII. [00073] 16.9 g of 3,3-Dimethyl-1-butanol (117.3 mmol) and 0.0382 g MeO-TEMPO (0.205 mmol) are charged in a jacketed glass reaction flask as in Example I. Sodium borate (0.380 g, 1.0 mmol) and 0.676 g NaHCO3 are dissolved in water (17 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 0 C. and the emulsion is re-adjusted to pH=8.4 using 50% solution of CH3COOH. When the temperature of the reactants reached 0 C., 77.5 g (126 mmol) of 12.1% aqueous NaOCl 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 few drops of 50% aqueous CH3COOH. The reaction mixture is stirred for an additional 120 min at 0 C. and the organic layer is sampled for GC assay. In this Example, 0.2-0.25 cc aqueous solution of NaOH (50% concentration) was added immediately after the bleach addition was completed and no efforts were made to maintain the pH of the emulsion. The yield of 3,3-dimethylbutyraldehyde is 94.0% at 60 min and 99.0% at 90 min reaction time

With the rapid development of chemical substances, we look forward to future research findings about 624-95-3.

Reference:
Patent; The NutraSweet Company; US6825384; (2004); B1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

624-95-3, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 624-95-3 as follows.

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 Zr (acetate) 2 (0.2 g solution, 0.1 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 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 95.0% at 60 min and 93.0% at 90 min reaction time.

The chemical industry reduces the impact on the environment during synthesis 624-95-3, I believe this compound will play a more active role in future production and life.

Reference:
Patent; THE NUTRASWEET COMPANY; WO2004/67484; (2004); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 624-95-3, name is 3,3-Dimethylbutan-1-ol. A new synthetic method of this compound is introduced below., 624-95-3

[00056] Example I represent a reference oxidation reaction under the conditions analogous to the one (reported in J.Organic Chemistry, 1987, 52, 2559 and J. Organic Chemistry, 1989, 54, 2970), also known as Anelli protocol. [00057] 820 mg of 3,3-Dimethyl-1-butanol (8 mmol) and 14.9 mg MeO-TEMPO (0.08 mmol) are dissolved in toluene (20 cc) in a jacketed glass reaction flask, equipped with a thermocouple, an addition port, a Teflon coated magnetic stir bar and a pH probe. Potassium bromide (45.25 mg, 0.4 mmol) and 1310 mg of NaHCO3 are dissolved in water (21.6 cc) and the aqueous phase is added to the stirred organic fraction at 1000 RPM in the reaction flask. The stirred suspension is cooled to 0 C. and 5.4 g of 12.3% aqueous NaOCl (8.92 mmol) are added via a gas-tight syringe over 5 minutes. The reaction mixture is aged for an additional 30 min and the organic layer sampled for GC assay. The yield of 3,3-dimethylbutyraldehyde is 77% at 30 min and 91% at 60 min reaction time

At the same time, in my other blogs, there are other synthetic methods of this type of compound,624-95-3, 3,3-Dimethylbutan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; The NutraSweet Company; US6825384; (2004); B1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

624-95-3, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 624-95-3 as follows.

16.9 g of 3, 3-Dimethyl-l-butanol (117.3 mmol) and 0.0765 g MeO-TEMPO (0.411 mmol) are charged in a jacketed glass reaction flask, equipped with a thermocouple, an addition port, a Teflon coated magnetic stir bar and a pH probe. Potassium bromide (0.011 g, 0.104 mmol) and 0.676 g. NAHCO3 are dissolved in water (12.4 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 HCI. When the temperature of the reactants reached 0C, 82 g (133 mmol) of 12. 1% aqueous NAOCI solution are pumped in via a gas-tight syringe over 90 minutes. During the bleach addition, the pH is maintained at 8.3-8. 4 levels using few drops of 50% aqueous HCI. 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 is 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 89.7% at 60 min and 91.5% at 90 min reaction time.

The chemical industry reduces the impact on the environment during synthesis 624-95-3, I believe this compound will play a more active role in future production and life.

Reference:
Patent; THE NUTRASWEET COMPANY; WO2004/67484; (2004); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts