Month: January 2021

Related Products of 110-73-6 ,Some common heterocyclic compound, 110-73-6, molecular formula is C4H11NO, 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.

Reference Synthetic Example 19 tert-Butyl ethyl(2-hydroxyethyl)carbamate To a mixture of 2-(ethylamino)ethanol (8.91 g) and ethyl acetate (100 mL) was added di-tert-butyl dicarbonate (21.8 g) under ice-cooling. The reaction mixture was stirred at room temperature for 3 days, and washed with saturated brine, then, dried over anhydrous magnesium sulfate. The solution was concentrated under reduced pressure to give title compound as colorless oil (19.0 g). 1H-NMR (CDCl3): 1.11 (3H, t, J=7.0Hz), 1.47(9H,s), 3. 27 (2H, q, J=7. 0Hz), 3. 37 (2H, t, J=5.2Hz), 3. 73 (2H, q, J=5. 2Hz).

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. 110-73-6, 2-(Ethylamino)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP1602362; (2005); A1;,
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Synthetic Route of 19936-14-2, 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 19936-14-2, name is 1-(4-Bromophenyl)cyclobutanol. This compound has unique chemical properties. The synthetic route is as follows.

To a 50 mL two-neck flask were added 1-(4-bromophenyl)cyclobutanol (80 mg, 0.35 mmol), N-(1-((1-cyanocyclopropyl)carbamoyl)cyclohexyl)-6-(4,4,5,5 -tetramethyl-1,3,2-dioxaborolan-2-yl)benzofuran-2-carboxamide (168.0 mg, 0.35 mmol), Pd(dppf)Cl2¡¤CH2Cl2 (40 mg) and DMF (15 mL). To the mixture was added aqueous potassium carbonate (0.45 mL, 2 mol/L) under nitrogen protection. The resulting mixture was stirred at 90C for 3 h. To the reaction mixture was added saturated brine (50 mL), and the resulting mixture was extracted with ethyl acetate (50 mL*2). The combined organic layers were washed with saturated brine (40 mL*2), dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo, and the residue was purified by silica-gel column chromatography (DCM:EtOAc=4:1, V/V) to give a white solid (80 mg, 50%). MS(ESI, pos.ion)m/z:498.2 (M+1); 1H NMR (600 MHz, CDCl3) delta 8.16 (s, 1H), 7.77 (d, J= 10.6 Hz, 2H), 7.67 (dd, J= 20.5, 8.3 Hz, 4H), 7.61 (d, J = 8.2 Hz, 1H), 7.54 (s, 1H), 6.61 (s, 1H), 2.69 – 2.61 (m, 2H), 2.45 (dt, J = 12.5, 9.5 Hz, 2H), 2.28 (d, J = 13.8 Hz, 2H), 2.15 – 1.98 (m, 5H), 1.82 – 1.72 (m, 4H), 1.55 (dt, J = 24.7, 9.6 Hz, 4H), 1.26 – 1.23 (m, 2H).

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 19936-14-2, 1-(4-Bromophenyl)cyclobutanol.

Reference:
Patent; Sunshine Lake Pharma Co., Ltd.; WANG, Xiaojun; ZHOU, Pingjian; YANG, Chuanwen; HUANG, Changwei; XIONG, Shaohui; ZHANG, Yingjun; ZHANG, Jiancun; (139 pag.)EP3342765; (2018); 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. 4461-39-6, name is N-(2-Hydroxyethyl)-1,3-propanediamine. A new synthetic method of this compound is introduced below., category: alcohols-buliding-blocks

To a round-bottom flask (250 mL) containing 3-(benzyloxy)benzaldehyde (3.50 g, 16.5 mmol) dissolved in methanol (100 ml), N-(2-Hydroxyethyl)-1,3-propanediamine (3.50 g, 16.5 mmol) was added. The resulting mixture was stirred for 2 h at ambient temperature. Then carbon disulfide (1.00 mL, 16.5 mmol) was slowly mixed to the reaction, which was kept under stirring for about 40 min. Cu(O2CCH3)2H2O (1.50 g, 8.25 mmol) was then added and a brown solid was formed. After stirring for 4 h, the formed brown precipitate was filtrated and re-crystallized in a 4:1 mixture of CH2Cl2 and toluene. Yield 81%. Mp. 93.6-95.0 C. IR (cm-1, KBr): 1496 (nuN-CS); 980 {nuasym(C-S)}; 601 {nusym(C-S)}. Analysis of C, H and N, respectively for C40H48N4O4S4Cu found% (calc.%): 56.95 (57.15); 5.67 (5.76); 6.58 (6.66).

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, 4461-39-6, N-(2-Hydroxyethyl)-1,3-propanediamine.

Reference:
Article; Ferreira, Isabella P.; Lima, Geraldo M. De; Paniago, Eucler B.; Takahashi, Jacqueline A.; Krambrock, Klaus; Pinheiro, Carlos B.; Wardell, James L.; Visentin, Lorenzo C.; Journal of Molecular Structure; vol. 1048; (2013); p. 357 – 366;,
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Related Products of 60211-57-6, 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. 60211-57-6, name is 3,5-Dichlorobenzyl alcohol. A new synthetic method of this compound is introduced below.

To a solution of 3.5 g of 3,5-dichlorobenzyl alcohol (Aldrich) in 75 mL of dichloromethane at 0C was added 1.8 mL of methane sulfonylchloride followed by 3.5 mL of triethylamine added dropwise. After 2 hours the solution was diluted to 150 mL with dichloromethane, washed with 3N HCl, saturated aqueous NaHCO3 dried with Na2SO4 and the solvents removed to yield the desired 3,5-dichlorobenzyl methanesulfonate as a yellow oil that was used without purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,60211-57-6, 3,5-Dichlorobenzyl alcohol, and friends who are interested can also refer to it.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; ELI LILLY AND COMPANY; EP951466; (2009); B1;,
Alcohol – Wikipedia,
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Related Products of 115-20-8 ,Some common heterocyclic compound, 115-20-8, molecular formula is C2H3Cl3O, 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.

To a stirring solution of 5-chloro-2-(quinolin-6-yl)benzoic acid (0.201 g, 0.708 mmol) and TEA (0.148 ml, 1.06 mmol) in 1 ,4-dioxane (10 ml) at RT, was added DPPA (0.191 ml, 0.244 mmol). After stirring for 30 min at RT, 2,2,2-trichloroethanol (0.680 ml, 7.08 mmol) was added and the reaction was stirred with heating at 100 C for 2 h. The completed reaction was diluted with brine (10 ml) and extracted with EtOAc (3×25 ml). The combined organics were washed with 5% citric acid (10 ml), sat’d. NaHC03 (10 ml) and brine (10 ml), dried (MgSO^, concentrated in vacuo and purified by chromatography to afford 2,2,2-trichloroethyl 5-chloro-2-(quinolin-6- yl)phenylcarbamate (0.25 g, 82% yield) as a white solid. MS (ESI) m/z: 431.0 (M+H+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,115-20-8, its application will become more common.

Reference:
Patent; DECIPHERA PHARMACEUTICALS, LLC; FLYNN, Daniel L.; PETILLO, Peter A.; KAUFMAN, Michael D.; WO2013/36232; (2013); A2;,
Alcohol – Wikipedia,
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Related Products of 4152-92-5 , The common heterocyclic compound, 4152-92-5, name is (2-(Aminomethyl)phenyl)methanol, molecular formula is C8H11NO, 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.

An ice-cold pyridine solution (10 mL) of compound 23 (1 mmol) is treated successively, in a dropwise fashion with acetyl chloride (1 mmol), then after 5 min with MsCl (1.1 mmol). The solution is warmed to room temperature then the solvent is removed. The residue is dissolved in EtOAc, washed with water, dried (MgS04), filtered and concentrated in vacuo. Purification by column chromatography affords pure compound 24.

The synthetic route of 4152-92-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ONTORII, INC.; BUTLER, David; IWAMOTO, Naoki; MEENA, Meena; SVRZIKAPA, Nenad; VERDINE, Gregory L.; ZLATEV, Ivan; WO2014/12081; (2014); A2;,
Alcohol – Wikipedia,
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Reference of 86770-74-3 ,Some common heterocyclic compound, 86770-74-3, molecular formula is C8H19NO4, 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.

An oven-dried 200 mL round bottomed flask was charged with Biotin-NHS (1.17 g, 3.43 mmol) and 2-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)ethan-1-ol (730 mg, 3.80 mmol). The flask was subjected to three cycles of vacuum/nitrogen backfill before addition of anhydrous DMF (69 mL). To the colorless solution was added triethylamine (960 muL, 6.85 mmol) and after 45 minutes, the solution was concentrated in vacuo. The crude material was purified by flash chromatography (basic alumina: 5 % methanol in CH2Cl2) to provide the title compound as an opaque amorphous solid (1.18 g, 2.81 mmol, 82 % yield). 1H NMR (400 MHz, CDCl3) delta: 7.21 (1H, br t), 5.97 (1H, br s), 5.09 (1H, br s), 4.48 (1H, m), 4.30 (1H, m), 3.78 (1H, m), 3.70 (4H, m), 3.65-3.58 (8H, m), 3.52 (2H, m), 3.41 (2H, m), 3.13 (1H, td, J = 7.4, 4.6 Hz), 2.90 (1H, dd, J = 12.8, 5.0 Hz), 2.73 (1H, d, J = 12.8 Hz), 2.20 (2H, t, J = 7.5 Hz), 1.78 (4H, m), 1.46-1.38 (2H, m); 13C NMR (100 MHz, CDCl3) delta: 173.49, 164.17, 72.60, 70.51, 70.32, 70.17, 70.00, 69.92, 61.78, 61.41, 60.22, 55.65, 40.47, 39.08, 35.90, 28.30, 28.11, 25.69. IR numax/cm-1 (film): 3273, 3085, 2916, 2865, 1690, 1669, 1646, 1551, 1464, 1420, 1264, 1240, 1202, 1101, 869, 693. m/z HRMS (ESI): [M+ H]+ calculated for C18H33N3O6S+ = 442.1982, found 442.1962.

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. 86770-74-3, 2-(2-(2-(2-Aminoethoxy)ethoxy)ethoxy)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Nottingham, Kyle G.; McNally, Andrew; McNaughton, Brian R.; Tetrahedron Letters; vol. 59; 3; (2018); p. 234 – 237;,
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Adding a certain compound to certain chemical reactions, such as: 32328-03-3, Diethyl 3-hydroxyglutarate, 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, 32328-03-3, blongs to alcohols-buliding-blocks compound. Safety of Diethyl 3-hydroxyglutarate

Sodium hydroxide (0.80 g, 20 mmol) was dissolved in water (10 mL), diethyl 3-hydroxyglutarate (0.95 g, 5.0 mmol) was added thereto, and the mixture was stirred at room temperature for 1 hour. Next, after cooling the reaction solution on ice,65% nitric acid was added in an equimolar amount to sodium hydroxide and stirred for 1 hour under ice cooling. to this, An aqueous solution (0.70 mL) containing silver nitrate (1.70 g, 10 mmol) was added dropwise and the mixture was further stirred for 1 hour. Thereafter, the precipitated white precipitate was collected by filtration.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,32328-03-3, its application will become more common.

Reference:
Patent; NOF CORPORATION; TAGAMI, YASUNOBU; MORISHITA, TAKEHIRO; MICHINISHI, JUNYA; (16 pag.)JP2015/107938; (2015); A;,
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Electric Literature of 57772-50-6 ,Some common heterocyclic compound, 57772-50-6, molecular formula is C8H11NO, 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.

General procedure: To an oven-dried 15 mL sealed tube were added 2-aminophenylmethanol 1 (0.425 mmol), benzonitrile 2(0.25 mmol), Ru cat. b (1.94 mg, 1 mol%), and KOtBu (14.02 mg, 0.5equiv) intamyl alcohol (1 mL) under an air atmosphere. The sealedtube was capped and heated at 130C for 2 h. The reaction mixturewas cooled down to room temperature and directly concentratedunder vacuum. The crude mixture was puried by preparative thin-layer-chromatography (petroleum ether/ethyl acetate 20/1) togive the desired product 3 or 4.

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. 57772-50-6, (2-Amino-3-methylphenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wan, Xiao-Min; Liu, Zi-Lin; Liu, Wan-Qing; Cao, Xiao-Niu; Zhu, Xinju; Zhao, Xue-Mei; Song, Bing; Hao, Xin-Qi; Liu, Guoji; Tetrahedron; vol. 75; 18; (2019); p. 2697 – 2705;,
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Adding a certain compound to certain chemical reactions, such as: 311-86-4, 2-Bromo-3,3,3-trifluoropropan-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, Quality Control of 2-Bromo-3,3,3-trifluoropropan-1-ol, blongs to alcohols-buliding-blocks compound. Quality Control of 2-Bromo-3,3,3-trifluoropropan-1-ol

54 g of 2-bromo-3,3,3-trifluoropropanol, 79 g of methanol, 9.7 g of activated RaneyNi catalyst and 19.3 g of potassium carbonate were charged into a 300 mL autoclave, stirred, evacuated and replaced with hydrogen After three times, pressure 5Mpa, heated to 80 C, the reaction 3.0h, stop the reaction, cooling, discharge, distillation to 3,3,3 – trifluoropropanol; Yield 95.0%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,311-86-4, 2-Bromo-3,3,3-trifluoropropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; Xi’an Modern Chemistry Research Institute; Gu, Yujie; Lu, Jian; Ma, Hui; Wang, Zhixuan; Kang, Jianping; Du, Yongmei; Tu, Donghuai; Wan, Hong; Li, Yang; (5 pag.)CN105399607; (2016); A;,
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