Author: tianli

Synthetic Route of 13330-96-6, 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. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol, molecular formula is C6H15NO, 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 mixture of sodium hydride (72%, 232 mg, 7.0 mmol) and tetrahydrofuran (20 ml) was added 4-(dimethylamino)-1-butanol (0.82 g, 7.0 mmol) at 0C (external temperature), and the reaction mixture was stirred at 45C for 20 minutes. Then, the reaction mixture was cooled at 0C (external temperature). To the reaction mixture was added dropwise a mixture of tributyl-iodomethyl-tin (2.0 g, 4.6 mmol) and N,N-dimethylformamide (20ml) at the same temperature. Then, the reaction mixture was stirred at 45C for 30 minutes. The reaction mixture was brought to room temperature, water and ethyl acetate were added to the reaction mixture, and the organic layer was separated. The organic layer was washed with water and an aqueous saturated sodium chloride solution, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (heptane: ethyl acetate=20:1, NH silica gel) to obtain the title compound (1.4 g, 3.3 mmol, 70%). 1H-NMR Spectrum (CDCl3) delta (ppm) : 0.81-0.97 (15H, m), 1.26-1.35(6H, m), 1.47-1.55(10H, m), 2.21(6H, s), 2.24-2.28(2H, m), 3.30-3.33(2H, m), 3.71(2H, t, J=6.8Hz).

According to the analysis of related databases, 13330-96-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Eisai R&D Management Co., Ltd.; EP1867650; (2007); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 27489-62-9, trans-4-Aminocyclohexanol, 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, Recommanded Product: 27489-62-9, blongs to alcohols-buliding-blocks compound. Recommanded Product: 27489-62-9

Step -I: trans-4-(Dibenzylamino)cyclohexanol (intermediate B8-1) [00288] Benzyl bromide (11.36 mL, 96 mmol) was subsequently added dropwise to a stirring solution of trans -4-aminocyclohexanol (5 g, 43.4 mmol) and potassium carbonate (21g, 152 mmol) in acetonitrile (100 mL). The reaction mixture was stirred at 90 C for 16 h, cooled to ambient temperature, filtered through a Celite pad, and washed with ethyl acetate. The filtrate was concentrated in vacuo. The residue was purified using CombiFlash (40.0 g silica gel column; 2% methanol in DCM), to obtain the title product (6 g, 20.31 mmol, 46.8% yield), as an off-white solid. lU NMR (400 MHz, chloroform-d) delta 7.34 – 7.38 (m, 4H), 7.26 – 7.31 (m, 4H), 7.15 – 7.24 (m, 2H), 3.61 (s, 5H), 2.52 (s, 1.96 – 2.06 (m, 2H), 1.88 (br. s., 2H), 1.43 (d, J= 15.31 Hz, 2H), 1.21 (br. s., 2H); MS(ES): m/z 296.2 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,27489-62-9, trans-4-Aminocyclohexanol, and friends who are interested can also refer to it.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WASHBURN, William N.; MURUGAIAH SUBBAIAH, Murugaiah Andappan; AHMAD, Saleem; WO2014/39412; (2014); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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. 623-50-7, name is Ethyl 2-hydroxyacetate, molecular formula is C4H8O3, 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. SDS of cas: 623-50-7

A solution of ethyl glycolate (500 mg, 4.8 mmol) and tosyl chloride (915 mg, 4.8 mmol) in anhydrous diethyl ether (2 ml) at 0 0C was treated dropwise with triethylamine (1.34 ml, 9.6 mmol). The temperature was maintained at 0 0C with stirring for a further 2 h. After this time, water was added and the phases separated. The aqueous phase was extracted with fresh diethyl ether. The combined organic extracts were dried (MgSO4), filtered and the solvent removed in vacuo. The crude product was purified by column chromatography over silica gel (Rf=0.29, 25% ethyl acetate in hexane) affording the tosylate 2 as a colorless oil which solidified on standing as a white solid (868 mg, 70%). [This procedure was repeated on 2 x scale (1.8 g, 73%)]. deltaH (400 MHz, CDCl3) 1.22-1.27 (3H, m, CH3), 2.46 (3H, s, ArCH3), 4.16-4.22 (2H, m, CH2CH3), 4.58-4.59 (2H, m, OCH2), 7.36 (2H, d, J=8.2 Hz, ArH), 7.84 (2H, d, J=8.2 Hz, ArH); deltac (100.6 MHz, CDCl3) 14.2, 21.9, 62.1, 64.9, 128.3,130.1, 132.9, 145.5, 166.2; MS (ES+) 276.0 (100%, [M+H20]+) (ion not detected in ES’).

With the rapid development of chemical substances, we look forward to future research findings about 623-50-7.

Reference:
Patent; H. LEE MOFFITT CANCER CENTER & RESEARCH INSTITUTE; UNIVERSITY OF SOUTH FLORIDA; UNIVERSITY OF CENTRAL FLORIDA; WO2007/136858; (2007); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 7397-62-8, Butyl 2-hydroxyacetate, 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, SDS of cas: 7397-62-8, blongs to alcohols-buliding-blocks compound. SDS of cas: 7397-62-8

47.6 g (0.5 mol) of phenol, 134.2 g (1.04 mol) of butyl hydroxyacetate, and 0.36 g of catalyst Mo2P5-MCM-48 (molar ratio of Mo1P3 and MCM-48: 25:100) were mixed and stirred, and the temperature was raised to 100-120 C, the rectification water was reacted for 2 hours in this process. When the top of the column is substantially anhydrous, the reaction is completed, the temperature is lowered to room temperature, the catalyst is removed by suction filtration, the catalyst is continuously activated after the catalyst is activated, the obtained mother liquid is distilled to recover the solvent, and then the unsubstituted butyl hydroxyacetate and phenol are separated by distillation to obtain the product benzene. Butyl oxyacetate 69.6 g, purity 98.2%, selectivity 99.2%, yield 65.78%. The prepared butyl phenoxyacetate was detected by nuclear magnetic resonance, and the nuclear magnetic resonance spectrum was as shown in Fig. 2.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,7397-62-8, Butyl 2-hydroxyacetate, and friends who are interested can also refer to it.

Reference:
Patent; Shandong Runbo Biological Technology Co., Ltd.; Sun Guoqing; Hou Yongsheng; Chi Zhilong; He Enjing; Hu Yishan; (8 pag.)CN108947841; (2018); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Electric Literature of 42514-50-1, 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. 42514-50-1, name is 3-Amino-3-methylbutan-1-ol. A new synthetic method of this compound is introduced below.

Component XI [preparation of the compound of formula (IIIb)]N-tert-butoxycarbonyl-4,4-dimethyl-[1,2,3]oxathiazinane-2,2-dioxide a. tert-butyl (3-hydroxy-1,1-dimethylpropyl)-carbamidate 3-amino-3-methylbutan-1-ol (200.0 g, 1.94 mol) is dissolved in ethyl acetate (0.75 l) and within one hour combined with a solution of di-tert-butyl-dicarbonate (435.0 g, 1.99 mol) in ethyl acetate (0.75 l). After the addition has ended the reaction mixture is stirred for another 30 min. After elimination of the solvent the title compound is obtained, which is used in the next step without further purification. Yield: 412.5 g 1H-NMR (DMSO, 400 MHz): 1.19 (s, 9H); 1.36 (s, 6H); 1.68-1.74 (m, 2H); 3.42-3.50 (m, 2H); 4.39 (t, J=4.8, 1H); 6.36 (br s, 1H). Alternatively tert-butyl (3-hydroxy-1,1-dimethylpropyl)-carbamidate may also be prepared using the methods described for example in J. of Labell. Compounds & Radioph. 2001, 44(4), 265-275 or der WO 03/037327, p. 82/83.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,42514-50-1, its application will become more common.

Reference:
Patent; Walter, Rainer; Hamilton, Bradford S.; Trieselmann, Thomas; Netherton, Matthew R.; Santagostino, Marco; Konetzki, Ingo; US2007/105906; (2007); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Electric Literature of 2002-24-6, 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 2002-24-6 as follows.

EXAMPLE 2 N-(3-{4-[3-Chloro-4-(3-fluoro-benzyloxy)-phenylamino]-quinazolin-6-yl}-prop-2-ynyl)-N’-cyano-N”-3-(2-hydroxy-ethyl)guanidine. A mixture of crude 1-(3-{4-[3-chloro-4-(3-fluoro-benzyloxy)-phenylamino]-quinazolin-6-yl}-prop-2-ynyl)-2-phenyl-N-cyano-isourea (70 mg, 0.12 mmol) (from Step H, Example 1), 2-hydroxyethylamine hydrochloride (39 mg, 0.4 mmol) and triethylamine (0.07 mL, 0.5 mmol) in isopropanol (2 mL) was heated to 85 C. in a sealed tube. The reaction was cooled to room temperature after 3 hours. Solvent was removed via rotovap. The residue was then purified by FCC to give the final productproduct (25 mg, 38%) as a light yellow solid. MS ESI (+) m/z 544 (M+1) detected; 1H NMR (400 MHz, deuterated DMSO) 9.95 (s, 1H), 8.7 (s, 1H), 8.6 (s, 1H), 8.05 (s,1H), 8.0 (s, 1H), 7.8 (m, 1H), 7.78 (m, 2H), 7.6 (br, 1H), 7.5 (m, 1H), 7.22-7.4 (m, 2H), 7.2 (m, 1H), 7.1 (m, 1H), 5.25 (s, 2H), 4.25 (m, 2H), 3.5 (m, 2H), 3.25 (m, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2002-24-6, its application will become more common.

Reference:
Patent; Wallace, Eli; Topolov, George; Zhao, Qian; Lyssikatos, Joseph P.; US2005/101617; (2005); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Electric Literature of 2615-15-8, 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 2615-15-8 as follows.

1005671 A solution of hexaethylene glycol (10 g, 35.46 mmol) in DCM (100 mL) was charged with Ag20 (12.34 g, 53.19 mmol), KI (1.17 g, 7.04 mmol) and stirred at room temperature for 15 mm. This solution was charged with tosyl chloride (7.35 g, 38.68 mmol)and stirred at room temperature for 6 h. The reaction mixture was filtered through a pad of celite and the filtrate was concentrated in vacuo resulting in a crude compound which was purified by chromatography on silica gel, eluting with 2% methanol in DCM to give 8.80 g, 57% yield of the title compound as colorless oil. ?H NMR (400 MHz, DMSO-d6): oe = 7.78 (d, J= 7.9 Hz, 2H), 7.48 (d, J= 7.7 Hz, 2H), 4.56 (t, J= 5.4 Hz, 1H), 4.11 (t, J= 4.3 Hz, 2H), 3.563.32 (m, 22H), 2.42 (s, 3H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2615-15-8, its application will become more common.

Reference:
Patent; COFERON, INC.; FOREMAN, Kenneth, W.; JIN, Meizhong; WANNER, Jutta; WERNER, Douglas, S.; WO2015/106292; (2015); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Electric Literature of 612-16-8, 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 612-16-8, name is (2-Methoxyphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The mixture of benzyl alcohol (1a, 0.3244 g, 3.0 mmol,1.5 equiv.), 2-aminopyridine (6a, 0.1882 g, 2.0 mmol), and NaOH (0.0400 g, 1.0 mmol, 50 mol%)was sealed under air in a 20 mL Schlenk tube and then stirred at 150 oC for 24 h. After completion,the reaction was monitored by TLC and/or GC-MS (>99% GC conversion) and the crude productwas purified by column chromatography using ethyl acetate and petroleum ether as eluent. Thetarget product 7a was obtained in 89% isolated yield. White solid. 1H NMR (500 MHz, CDCl3): delta 8.10 (dd,J = 5.0 Hz, J = 1.0 Hz, 1H), 7. 39-7.36 (m, 1H), 7.31 (d, J = 7.5 Hz, 1H), 7.26-7.23 (m, 1H),6.92-6.87 (m, 2H), 6.56-6.54 (m, 1H), 6.39 (d, J = 7.5 Hz, 1H), 5.01 (b, 1H), 4.48 (d, J = 6.0 Hz,2H), 3.85 (s, 3H). 13C NMR (125.4 MHz, CDCl3): delta 158.9, 157.4, 148.2, 137.3, 128.8, 128.3, 127.1,120.5, 112.8, 110.2, 106.7, 55.3, 41.7. MS (EI): m/z (%) 214 (60), 183 (92), 136 (45), 121 (35), 105(31), 91 (100), 78 (48), 65 (25), 51 (14).

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 612-16-8, (2-Methoxyphenyl)methanol.

Reference:
Article; Li, Xiaohui; Li, Shuangyan; Li, Qiang; Dong, Xu; Li, Yang; Yu, Xiaochun; Xu, Qing; Tetrahedron; vol. 72; 2; (2016); p. 264 – 272;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 42514-50-1, 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 42514-50-1, name is 3-Amino-3-methylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

Step 4: (3-Hydroxy-1,1-dimethyl-propyl)-carbamic acid tert-butyl ester. 3-Amino-3-methyl-butan-1-ol(5.0 g, 0.04 mol) was dissolved in 150 mL CH2Cl2 and treated with di-tert-butyl dicarbonate(11.12 g, 0.05 mol). The resulting mixture was stirred for 18 h at 25 C. The mixture was concentrated to the desired material as an amber oil(9.8 g, 100%); 1H NMR (DMSO-d6) delta 3.55 (s,1H), delta 4.43 (t, J=5 Hz, 1H), delta 3.46 (m, 2H), delta 1.71 (t, J=7 Hz, 2H), delta 1.37(s, 9H), delta 1.12(s, 6H).

According to the analysis of related databases, 42514-50-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Kim, Kyoung S.; Lu, Songfeng; Sheng, X. Christopher; Crews JR., Alvin Donald; US2004/242596; (2004); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts