Month: July 2021

Reference of 1072-52-2, 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. 1072-52-2, name is 2-(Aziridin-1-yl)ethanol. A new synthetic method of this compound is introduced below.

Example 10 (Table 1, entry 4 and Scheme 7): Preparation of 2- [(2-iodoethyl)-2,4- dinitro-6-({[2-(tetrahydro-2/£pyran-2-yloxy)ethyl]amino}carbonyl)anih’no]ethyl methanesulfonate (17c); A slurry of 15 (520 mg, 1.4 mmol) in dry 3-methyl-2-butanone (20 mL) and NaI (3.1 g) was cooled to below 5 0C, and aziridineethanol (240 mg, 2.76 mmol) was added. The reaction was kept at 20 0C overnight, then water (100 mL) was added, and the mixture was extracted with EtOAc (3×50 mL). The combined organic layer was washed with water, dried and concentrated under pressure, then passed through a short column of silica gel, eluting with heptane/EtOAc (1:1), to give 2-[(2-hydroxyethyl)(2-iodoethyl)amino]-3,5- dinitro-N-[2-(tetrahydro-2H-pyran-2-yloxy)ethyl]benzamide (16c) (630 mg, 82%) as a yellow foam; 1H NMR (CDCl3) delta 8.63 (d, / = 2.8 Hz, 1 H), 8.56 (dj = 2.8 Hz, 1 H), 8.24 (br, 1 H), 4.54 (m, 1 H), 4.48 (m, 1 H), 3.93 (m, 2 H), 3.84 (m, 1 H), 3.70 (m, 6 H), 3.54 (m, 1 H), 3.30 (m, 2 H), 3.18 (m, 2 H), 1.90-1.40 (m, 6 H); 13C NMR delta 165.7, 146.7, 144.4, 140,9, 134.5, 129.2, 123.5, 101.6, 67.0, 65.4, 58.0, 55.0, 53.7, 40.7, 31.3, 25.1, 21.2, 0.3; HRMS (FAB) calcd for C18H26IN4O8 [MH]+ m/z 553.0795; found 533.0797.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,1072-52-2, 2-(Aziridin-1-yl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; AUCKLAND UNISERVICES LIMITED; WO2008/30112; (2008); A1;,
Alcohol – Wikipedia,
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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. 33524-31-1, name is (2,5-Dimethoxyphenyl)methanol. A new synthetic method of this compound is introduced below., Product Details of 33524-31-1

Example 10; 5-Chloro-1-(2,5-dimethoxybenzyl)-1H-indole-2-carboxylic acid (3-hydroxy-2,2- dimethylpropyDamide EPO A solution of phosphorous tribromide (5.74ml, 60.4mmol) in anhydrous DCM (90ml) was added over 20min to a cooled, stirred solution of 2,5-dimethoxybenzyl alcohol (25.Og, 148.8mmol) in DCM (180ml), maintaining the temperature between -5C and 00C. Following the addition, the reaction was stirred at this temperature for a further 20 min. when water (200ml) was added. After separation of the layers, the organic was washed with water (3x200ml), dried with magnesium sulfate and evaporated to dryness under reduced pressure. The resulting crude product was crystallised from diethyl ether/heptane to afford 2-bromomethyl-1,4-dimethoxy-benzene (24.2g, 72%).The title compound was then prepared in a manner similar to that described in Example 1. 1H NMR (400MHz, CDCI3) deltaH : 0.88(s, 6H), 3.08(d, 2H, J=7.0), 3.25(d, 2H, J=6.8), 3.52(t, 1 H, J=7.0), 3.57(s, 3H), 3.84(s, 3H), 5.75(s, 2H), 6.03(d, 1H, J=2.9), 6.59(br t, 1H, J=6.8), 6.68(dd, 1 H, J=8.8, 2.9), 6.80(d, 1 H, J=8.8), 6.85 (s, 1H), 7.19(dd, J=8.8, 1.9), 7.27(m, 1H), 7.60(d, 1 H, J=1.9); EIMS: m/z = 431.3 [M+H]+.

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, 33524-31-1, (2,5-Dimethoxyphenyl)methanol.

Reference:
Patent; N.V. ORGANON; WO2006/100208; (2006); A1;,
Alcohol – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 7417-18-7, 2-(2-Methoxyphenyl)ethanol, 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, Application In Synthesis of 2-(2-Methoxyphenyl)ethanol, blongs to alcohols-buliding-blocks compound. Application In Synthesis of 2-(2-Methoxyphenyl)ethanol

b) 4-Bromo-2-(2-hydroxyethyl)-anisole 35.72 g of tetrabutylammonium tribromide am added in portions to a solution of 10.7 g of 2-(2-hydroxyethyl)-anisole in 195 ml of dichloromethane and 130 ml of methanol. The reaction mixture is stirred for 150 minutes at room temperature and is then concentrated by evaporation in a rotary evaporator. The residue is partitioned between diethyl ether and water. The organic phases are combined, dried over magnesium sulfate and concentrated by evaporation, and the residue is purified by means of FC (dichloromethane), yielding the title compound: Rf (dichloromethane)=0.26; HPLC Rt =13.04 minutes.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,7417-18-7, 2-(2-Methoxyphenyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; Ciba-Geigy Corporation; US5559111; (1996); A;,
Alcohol – Wikipedia,
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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. 5391-88-8, name is 1-(4-Bromophenyl)ethanol, molecular formula is C8H9BrO, 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. name: 1-(4-Bromophenyl)ethanol

General procedure: Under an N2 atmosphere, a mixture of secondary alcohol (0.5 mmol), primary alcohol (0.6 mmol), 1a (5 mol %), NaOH (0.1 mmol), 4 A molecular sieve (0.6 g), and toluene (1.5 mL) was added into a 25 mL Schlenk tube equipped with a stirring bar. The mixture was heated to 120 C under a slow and steady N2 flow for 24 h. After cooling to ambient temperature, 6 mL water was added and the aqueous solution extracted with ethyl acetate (3 x 5 mL). The combined extracts were dried over anhydrous Na2SO4, and concentrated under reduced pressure. The crude product purified on a short flash chromatography column.

With the rapid development of chemical substances, we look forward to future research findings about 5391-88-8.

Reference:
Article; Zhang, Shi-Qi; Guo, Bin; Xu, Ze; Li, Hong-Xi; Li, Hai-Yan; Lang, Jian-Ping; Tetrahedron; vol. 75; 47; (2019);,
Alcohol – Wikipedia,
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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. 42514-50-1, name is 3-Amino-3-methylbutan-1-ol. A new synthetic method of this compound is introduced below., category: alcohols-buliding-blocks

vTn a glass RBF equipped with a Teflon-coated magnetic stirrer was combined 4-fluoro-1,2-dinitrobenzene (1 eq.), 3- amino-3-methylbutan-1-ol (1 eq.) and ethyl diisopropyl amine (1.5 eq.) in DMSO (0.5 M). The resulting mixture was then heated at 100C for 24 h. The reaction mixture was then diluted with water and extracted with EtOAc. The combined organic extracts were washed further with water and brine, dried over MgSO4, filtered and the filtrate concentrated in vacuo. Further purification of the crude product thus obtained by way of column chromatography (Si02, gradient elution, 9:1 (v/v) Hex: EtOAc – EtOAc) furnished the desired product (22% yield).

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, 42514-50-1, 3-Amino-3-methylbutan-1-ol.

Reference:
Patent; MERCK PATENT GMBH; JORAND-LEBRUN, Catherine; LAN, Ruoxi; CHEN, Austin; CLARK, Ryan C.; (268 pag.)WO2017/49068; (2017); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 19064-18-7 ,Some common heterocyclic compound, 19064-18-7, molecular formula is C7H6F2O, 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.

A mixture of (2,6-difluorophenyl)methanol (1 mL) and sodium hydride (60%, oil) (34 mg) was stirred at room temperature for 30 min. 3-(4-Chloropyridin-2-yl)quinazoline-2,4(1H,3H)-dione (115 mg) was added, and the obtained mixture was stirred at 150C for 4 hr. The reaction mixture was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (31 mg). 1H NMR (300 MHz, DMSO-d6) delta 5.24 (2H, s), 7.14-7.31 (6H, m), 7.51-7.65 (1H, m),7.66-7.79 (1H, m), 7.87-8.06 (1H, m), 8.45 (1H, d, J = 5.7 Hz), 11.65 (1H, s).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,19064-18-7, its application will become more common.

Reference:
Patent; Takeda Pharmaceutical Company Limited; OGINO, Masaki; IKEDA, Zenichi; FUJIMOTO, Jun; OHBA, Yusuke; ISHII, Naoki; FUJIMOTO, Takuya; ODA, Tsuneo; TAYA, Naohiro; YAMASHITA, Toshiro; MATSUNAGA, Nobuyuki; EP2889291; (2015); A1;,
Alcohol – Wikipedia,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 61487-25-0, name is (2-Amino-3-chlorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of (2-Amino-3-chlorophenyl)methanol

EXAMPLE 100 Preparation of 2-benzyloxymethyl-6-chloroaniline This material was prepared from 2-amino-3-chlorobenzyl alcohol and benzyl bromide by the general procedure outlined in Example 98. The product was purified by Kugelrohr distillation to yield an oil, b.p. 118-125 C. (0.1 mm). The product was characterized by IR and 1 H NMR spectroscopy.

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, 61487-25-0, (2-Amino-3-chlorophenyl)methanol.

Reference:
Patent; The Dow Chemical Company; US4818273; (1989); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Application of 629-41-4, 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 629-41-4 as follows.

In a 2 L three-opening bottle into the 1, 8 – octandiol (250 g, 1.712 muM), toluene (1000 ml), 48% hydrogen bromide (231 ml, 2 . 054 muM, 1.2 eq), heating to 110 C reflux 30 hours. Added 48% hydrogen bromide (84 ml, 0 . 753 muM, 0 . 44 eq), heating reflux for 20 hours, GC detection with a small amount of residues of raw materials. Cooling to the room temperature plus 500 ml petroleum ether dilution, liquid […] bromic acid, organic phase are saturated sodium bicarbonate (400 ml × 2) and saturated brine (400 ml × 2) cleaning, dried with anhydrous sodium sulfate. Turns on lathe does 8 – bromine propyl butyl-carbinol 318 g, yield 83%, direct throws down the step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,629-41-4, its application will become more common.

Reference:
Patent; Changzhou University; He Jiayi; Xia Ran; Wu Linsheng; Hu Xiwen; Jin Xinyu; Chen Ke; Li Yuan; Qiu Lin; Chen Xin; (8 pag.)CN109796336; (2019); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 144-19-4, Adding some certain compound to certain chemical reactions, such as: 144-19-4, name is 2,2,4-Trimethyl-1,3-pentanediol,molecular formula is C8H18O2, 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 144-19-4.

238. 5g of 2, 2, 4-trimethyl-1, 3-pentanediol was placed (TMPD, 1.631 mol) in a 2-13- neck round-bottom flask. To this was added 205.7g DMC (2.283 mol, 40% excess) and 2.2g zinc stearate. The reaction flask was equipped with a thermocouple temperature probe, magnetic stirbar, and a 1″wide, 10″long vacuum-jacketed, silvered column packed with HastelloyG) B, atop which was placed a variable reflux K-head and condenser. The system was purged by bubbling nitrogen into the reaction mixture for 45 minutes prior to being heated. While under an atmosphere of nitrogen, the mixture was heated slowly to 100- 105C. After 30 minutes of heating, the boiling mixture began to reflux at an overhead temperature of 62-64C. The methanol byproduct/DMC azeotrope (typically a 70/30 wt/wt mixture of methanol/DMC) was removed at a reflux to takeoff ratio of between 3: 1 and 8: 1. After 2 hours of continuous heating, the temperature of the reaction mixture slowly began to rise, reaching 150-155C over the course of the next 15.5 hours as methanol was removed from the system. At this point, 37.9g DMC and 79.2g methanol (75.9% of total expected) had been removed from the reaction. The reaction mixture was then cooled to 60C and a vacuum was slowly introduced in order to remove unreacted DMC and additional methanol by-product. During this time, the temperature of the mixture was slowly increased. After 3 hours, the reaction mixture had been warmed to 90-95C and the system pressure had been reduced to 1.0-2. 0 mmHg. The system pressure was then further reduced to 0.5-1. 0 mmHg and the temperature of the mixture increased to 130C. Unreacted TMPD was preferentially removed from the reaction at an overhead temperature of 80-95C followed by distillation of the carbonate product 4-isopropyl-5, 5-dimethyl-1, 3-dioxan-2-one at an overhead temperature of 95-110C. Several cuts were taken during the distillation and analyzed by GC with the following results; Based on the above results (assuming actual wt. % is approximately equal to GC area %), reaction yield = 73.5%.

According to the analysis of related databases, 144-19-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; HUNTSMAN PETROCHEMICAL CORPORATION; WO2003/89424; (2003); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 34626-51-2, 5-Bromopentan-1-ol, 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, name: 5-Bromopentan-1-ol, blongs to alcohols-buliding-blocks compound. name: 5-Bromopentan-1-ol

Condensation of a-bromo aldehyde with 2,4-diamino-4-oxo-pyrimidine 19 is the key step in the synthesis of compounds 9-11 as outlined in Scheme 1 and Scheme 2. Commercially available alcohol 14 was coupled to the corresponding phenyl esters and oxidized to the corresponding aldehydes 17a and 17b (Scheme 1).-? Alcohol 24 was coupled to the appropriate phenyl ester to afford the aldehyde 25 (Scheme 2). The aldehydes were reacted with Br2 in dioxane to give the desired a-bromoaldehydes?2 18a, 18b (Scheme 1) and 26 (Scheme 2) and immediately reacted with 2,4-diamino-6-hydroxypyrimidine 19 to cyclize to the 5-substituted pyrrolo[2,3-d]pyrimidines 20a, 20b (Scheme 1) and 27 (Scheme 2).? Hydrolysis of the esters provided the free acids 21 a, 2 lb and 28. Subsequent peptide coupling with diethyl L-glutamate using the activating agents N-methyl morpholine and 2,4-dimethoxy-6-chlorotriazine, afforded the diesters 22a, 22b and 29. Saponification of the diesters yielded the final compounds 9-11 of this invention.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,34626-51-2, 5-Bromopentan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; DUQUESNE UNIVERSITY OF THE HOLY SPIRIT; WAYNE STATE UNIVERSITY; GANGJEE, Aleem; MATHERLY, Larry H.; (43 pag.)WO2016/22881; (2016); A1;,
Alcohol – Wikipedia,
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