Category: 2568-33-4

Related Products of 2568-33-4, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, molecular weight is 104.1476, as common compound, the synthetic route is as follows.

Under argon 3-methylbutane-1 ,3-diol (650 muIota_) is added at 0C to a suspension of NaH (ca. 60% in mineral oil; 400 mg). The mixture is stirred for 1 hour and then treated with 5-bromo-2-chloro-4,6-dimethylpyrimidine (1 .2 g). After stirring for 2 hours at room temperature the mixture is diluted with ethyl acetate and washed with ice- water and brine. After drying (MgSO4) the solvents are evaporated and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 70:39?50:50) to give the title compound. Yield: 1 .1 g; LC (method 3): tR = 0.79 min; Mass spectrum (EST): m/z = 289 [M+H]+.

Statistics shows that 2568-33-4 is playing an increasingly important role. we look forward to future research findings about 3-Methylbutane-1,3-diol.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ECKHARDT, Matthias; FRATTINI, Sara; HAMPRECHT, Dieter; HIMMELSBACH, Frank; LANGKOPF, Elke; LINGARD, Iain; PETERS, Stefan; WAGNER, Holger; WO2013/144098; (2013); A1;,
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Reference of 2568-33-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To a solution of 3-methylbutan-l,3-diol (10.0 g, 96.1 mmol) in DCM (100 mL) was added 4- methylbenzene- l-sulfonyl chloride (20.1 g, 106 mmol) and TEA (24.3 g, 240 mmol). The reaction mixture was stirred at room temperature for 12 h. Then the mixture was extracted with DCM (150 mLx3). The combined organic layers were washed with water and brine, dried over MgSC”4, and filtered. The filtrate was concentrated under reduced pressure. The resulting residue was purified by chromatography over silica gel (eluting with PE_EA=5: 1) to give the title compound.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 2568-33-4, 3-Methylbutane-1,3-diol.

Reference:
Patent; MERCK SHARP & DOHME CORP.; BIFTU, Tesfaye; COLLETTI, Steven L.; HAGMANN, William K.; KAR, Nam Fung; JOSIEN, Hubert; NAIR, Anilkumar; NARGUND, Ravi; BIJU, Purakkattle; ZHU, Cheng; HU, Bin; WO2015/51496; (2015); A1;,
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As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. COA of Formula: C5H12O2

5t (1.0 mmol), carbodiimide (CDI, 1.1 mmol), and DMAP(0.1 mmol) were sequentially added under air to a reaction tubeequipped with a stir bar and a septum. Et3N (1.5 mmol) and CH2Cl2(2 mL) was added by syringe and the resulting mixture vigorouslystirred for 3 h at ambient temperature. After this time, 8i(2.0 mmol) was sequentially added to this solution and the result-ing mixture again stirred for 14 h at ambient temperature. After thistime, the resulting solution was quenched with sat. NH4Claq andextracted with EtOAc. The solution obtained was ltered throughthe plug of silica gel and anhydrous MgSO4, and then concentratedby rotary evaporation. The pure product 9i was obtained byrecrystallization (65%, X mg, X mmol). IR(neat): 3484, 3341, 2970,1684, 1594, 1515, 1272, 1102 cm1.1H NMR (500 MHz, CDCl3) d: 8.59(brs, 1H), 8.02 (d, J 8.7 Hz, 2H), 7.63 (d, J 8.7 Hz, 2H), 4.49 (t,J 6.8 Hz, 2H), 2.05 (s, 6H), 1.98 (t, J 6.8 Hz, 2H), 1.32 (s, 6H);13CNMR (125 MHz, CDCl3) d: 170.30, 166.13, 141.66, 130.81, 126.32,119.23, 70.05, 62.49, 62.07, 41.80, 32.42, 29.81. HRESIMS calcd. forC16H23O4NBr (MH): 372.0810; found 372.0811.

With the rapid development of chemical substances, we look forward to future research findings about 2568-33-4.

Reference:
Article; Murata, Yumi; Takeuchi, Kentaro; Nishikata, Takashi; Tetrahedron; vol. 75; 18; (2019); p. 2726 – 2736;,
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Application of 2568-33-4, 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. 2568-33-4, name is 3-Methylbutane-1,3-diol. A new synthetic method of this compound is introduced below.

Step 1. Toluene-4-sulfonic acid 3-hydroxy-3-methyl-butyl ester 3-Methyl-1,3-butanediol (1.5 mL, 14.06 mmol) is suspended in dry dichloromethane (5 mL) and pyridine (1.24 mL, 15.46 mmol) is added followed by 4-toluenesulfonyl chloride (2.68 g, 14.06 mmol). The mixture is stirred overnight then washed with 1M aqueous hydrochloric acid, dried and the solvent removed under vacuum. The residue is purified by flash chromatography (0-30% ethyl acetate in cyclohexane) to give the title compound. (Yield 970 mg). LC (LC METHOD 4): tR=5.67 min; Mass spectrum (ES+): m/z=258 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; HAMPRECHT, Dieter; FRATTINI, Sara; LINGARD, Iain; PETERS, Stefan; US2013/324514; (2013); A1;,
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With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, molecular weight is 104.1476, as common compound, the synthetic route is as follows.Computed Properties of C5H12O2

To 3-methylbutane-1,3-diol (0.1 g, 0.98 mmol) was added potassium t-butoxide (0.94 mL, 1M in THF) and stirred for 10 minutes. Example 1E (0.2 g, 0.47 mmol) in 1.2 mL of THF was added and the mixture stirred at ambient temperature for 30 minutes. The mixture was diluted with dichloromethane, 20 muL of glacial acetic acid was added and the resulting mixture was filtered, loaded onto silica and chromatographed. (0-20% MeOH in dichloromethane (0.1% NH4OH) over 900 mL) to afford the title compound (70 mg, 0.14 mmol, 29% yield). 1H NMR (300 MHz, CDCl3) delta ppm 1.30 (s, 6H), 1.41 (s, 9H), 1.67-1.92 (m, 3H), 1.94-2.09 (m, 3H), 3.60-3.81 (m, 2H), 3.85 (s, 3H), 4.11-4.23 (m, 1H), 4.23-4.33 (m, 3H), 4.54 (dd, J=15.1, 2.9 Hz, 1H), 6.98 (d, J=8.5 Hz, 1H), 7.01 (s, 1H), 7.53 (dd, J=8.6, 2.2 Hz, 1H), 8.26 (d, J=2.4 Hz, 1H). MS (DCI/NH3) m/z 512.3 (M+H)+. Analytical calculated for C26H36F3N3O4.0.2H2O: C, 60.56; H, 7.13; N, 8.15. Found: C, 60.57; H, 7.25; N, 8.12

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; ABBOTT LABORATORIES; US2010/69348; (2010); A1;,
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With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, molecular weight is 104.1476, as common compound, the synthetic route is as follows.name: 3-Methylbutane-1,3-diol

[0153] 3-Methylbutane-1,3-diol (3.83 g, 36.8 mmol) wasdissolved in dichloromethane (150 ml), followed by the additionoftriethylamine(6.66 mL) andmethanesulfonyl chloride(3.13 mL) at oo C. After stirring at RT for7.5 hrs, the reactionwas quenched by ethyl acetate and water, and the organiclayer was dried over anhydrous sodium sulfate. The solventwas distilled off under reduced pressure to obtain the titlecompound as a colorless oil ( 4.79 g, 72%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2568-33-4, 3-Methylbutane-1,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; BLUEPRINT MEDICINES CORPORATION; Hodous, Brian L.; (150 pag.)US2016/31892; (2016); A1;,
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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. 2568-33-4, name is 3-Methylbutane-1,3-diol. A new synthetic method of this compound is introduced below., Application In Synthesis of 3-Methylbutane-1,3-diol

Example 19; Synthesis of Chain Transfer Agent; CTA-14.; 17 g (40 mmol) of 3-methyl-1,3-butanediol and 20.0 mL of tetrahydrofuran (THF) were weighed and placed in a 500 mL round bottom flask. The temperature of the system was adjusted to 25 C. and the mixture was stirred. After adding 18.98 g (240 mmol) of pyridine, 36.6 g (240 mmol) of S-acetyl mercaptoacetic acid chloride were added thereto dropwise over 30 minutes. After the addition, the mixture was aged at 25 C. for 5 hours. Subsequently, 20 mL of toluene and 20 mL of pure water were added thereto followed by stirring and the oil phase was concentrated. 35.0 g of the concentrate was weighed and placed in a 500 mL round bottom flask and 100 mL of methanol was added thereto. 200 mL of a saturated sodium bicarbonate solution was then added thereto dropwise over 30 minutes with cooling on an ice bath. Four hours after completion of the addition, 50 mL of pure water and 100 mL of ethyl acetate were added thereto and the mixture was stirred. The oil phase of the reaction solution was concentrated. The concentrate was recrystallized using hexane to give 5.04 g of CTA-1 shown below (yield 50%).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 2568-33-4, 3-Methylbutane-1,3-diol.

Reference:
Patent; Mitsubishi Rayon Co., Ltd.; US2009/198065; (2009); A1;,
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Synthetic Route of 2568-33-4, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.2568-33-4, name is 3-Methylbutane-1,3-diol, molecular formula is C5H12O2, molecular weight is 104.1476, as common compound, the synthetic route is as follows.

To a solution of 3-methylbutan-1, 3-diol (10.0 g, 96.1 mmol) in DCM (100 mL) was added 4-methylbenzene-1-sulfonyl chloride (20.1 g, 106 mmol) and TEA (24.3 g, 240 mmol) . The reaction mixture was stirred at room temperature for 12 h. Then the mixture was extracted with DCM (150 mL×3) . The combined organic layers were washed with water and brine, dried over MgSO4, and filtered. The filtrate was concentrated under reduced pressure. The resulting residue was purified by chromatography over silica gel (eluting with PE:EA5:1) to give the title compound.

The chemical industry reduces the impact on the environment during synthesis 2568-33-4, I believe this compound will play a more active role in future production and life.

Reference:
Patent; MERCK SHARP & DOHME CORP.; BIFTU, Tesfaye; BIJU, Purakkatle; COLLETTI, Steven L.; CUI, Mingxiang; HAGMANN, William K.; HU, Bin; JOSIEN, Hubert; KAR, Nam Fung; NAIR, Anilkumar; NARGUND, Ravi; SPERBECK, Donald M.; ZHU, Chen; WO2015/51725; (2015); A1;,
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Synthetic Route of 2568-33-4, Adding some certain compound to certain chemical reactions, such as: 2568-33-4, name is 3-Methylbutane-1,3-diol,molecular formula is C5H12O2, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2568-33-4.

Step 1: 4-Chloro-2-methyl-butan-2-ol 10.0 g (96.0 mmol)_3-methyl-1 ,3-butandiol is dissolved in 30.0 ml toluene and 10.7 g (106 mmol) TEA is added. The funnel is rinsed with 10.0 ml toluene. The mixture is heated to 80C and a mixture of 1 1 .6 g (101 mmol) methanesulfonyl chloride and 3.00 ml toluene is added. After complete addition, the funnel is rinsed with 7.00 ml toluene and the reaction mixture is heated to reflux for approx. 3h. After full conversion (GC) the mixture is cooled to 20 C and 40.0 ml water is added. Stirring is continued for a short period and the aqueous phase is separated. Then, approx. 10 ml of the organic phase is distilled off in vacuum. The crude toluene solution of the product is used for the next step.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 2568-33-4, 3-Methylbutane-1,3-diol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; DAHMANN, Georg; WAGNER, Holger; ECKHARDT, Matthias; FRANK, Markus; SANTAGOSTINO, Marco; SCHNAUBELT, Juergen; STERTZ, Uwe; PACHUR, Thorsten; WO2015/44073; (2015); A1;,
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Related Products of 2568-33-4, Adding some certain compound to certain chemical reactions, such as: 2568-33-4, name is 3-Methylbutane-1,3-diol,molecular formula is C5H12O2, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2568-33-4.

Toluene-4-sulfonic acid 3-hydroxy-3-methyl-butyl ester 3-Methyl-1,3-butanediol (1.5 mL, 14.1 mmol) is suspended in dry dichloromethane (5 mL) and pyridine (1.24 mL, 15.46 mmol) is added followed by 4-toluenesulfonyl chloride (2.68 g, 14.1 mmol). The mixture is stirred overnight then washed with 1 M aqueous hydrochloric acid, dried and the solvent removed under vacuum. The residue is purified by flash chromatography (0-30% ethyl acetate in cyclohexane) to give the title compound. (Yield 970 mg). LC (METHOD 2): tR=5.67 min; Mass spectrum (ES+): m/z=258 [M+H]+.

According to the analysis of related databases, 2568-33-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LINGARD, Iain; HAMPRECHT, Dieter; US2015/148347; (2015); A1;,
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