Month: March 2021

Electric Literature of 109-83-1, Adding some certain compound to certain chemical reactions, such as: 109-83-1, name is 2-(Methylamino)ethanol,molecular formula is C3H9NO, 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 109-83-1.

10 g (calculated on the basis of the dry substance) of a Pd-doped copper catalyst on active carbon (Degussa AG, CE 1015 OY/W) suspended in water was placed first analogously to example 1 in an autoclave and 61 g ethanolamine and 272 g sodium hydroxide solution (15% by weight) were added. The autoclave was closed and the contents were heated to 160 C. The pressure was kept at 12 bar (absolute) and the hydrogen that formed was continuously discharged by a pressure control valve. After the end of the reaction (which is evident from the decrease in gas release) it was cooled to 90 C. and the catalyst was removed from the product solution by filtration. 315 g filtrate which contained 29.8 g % by weight Na glycinate was obtained (corresponds to a yield of 96.7% of theory).The filtered catalyst was suspended in 10 g water and fed back into subsequent batches.

According to the analysis of related databases, 109-83-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Thalhammer, Franz; Gastner, Thomas; US2009/163739; (2009); A1;,
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Related Products of 15852-73-0 ,Some common heterocyclic compound, 15852-73-0, molecular formula is C7H7BrO, 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 50 {[(3-Bromophenyl)methyl]oxy}(1,1-dimethylethyl)dimethylsilane TBSCl (18.7 g, 124.3 mmol), Et3N (14.08 g, 139.2 mmol) and DMAP (194.3 mg, 8.9 mmol) were dissolved in CH2Cl2 (120 mL) and the solution was cooled to 0-5 C. (3-Bromophenyl)methanol (18.5 g, 99.4 mmol) was added dropwise to the solution. After the addition of the (3-Bromophenyl)methanol, the mixture was warmed to room temperature and stirred for 2 h. 5% HCl was added to the reaction mixture to adjust the pH=4-5. Then the organic phase was separated and the aqueous layer was extracted with CH2Cl2 (50 mL*2). The combined organic phases were washed with water and dried over Na2SO4. After removing the solvent, 28.5 g of {[(3-bromophenyl)methyl]oxy}(1,1-dimethylethyl)dimethylsilane was obtained (Yield: 95.1%).

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. 15852-73-0, (3-Bromophenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Glaxo Group Limited; US2009/203657; (2009); A1;,
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Electric Literature of 647-42-7, Adding some certain compound to certain chemical reactions, such as: 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol,molecular formula is C8H5F13O, 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 647-42-7.

Ways carboxylic acid (3d) can be synthesized by a known method, using the above shown illustrated by a compound (3c) was synthesized. In addition, the use of thionyl chloride to the carboxylic acid (3d) to the acid chloride derivative, gallic acid and so hydrate obtained by reacting a carboxylic acid (3e). The use of thionyl chloride acid (. 3E) to the acid chloride derivative, in the presence of DIPEA diol (3d) obtained by reacting the compound (24).

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. 647-42-7, 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Fuji Photo Film Co., Ltd.; Song, Shantashi; Jia, tengjunye; (56 pag.)CN104159996; (2016); B;,
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Application of 13674-16-3, 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.13674-16-3, name is Methyl 2-hydroxy-3-phenylpropanoate, molecular formula is C10H12O3, molecular weight is 180.2, as common compound, the synthetic route is as follows.

EXAMPLE 11 2-[4′-(2-Benzyl-benzofuran-3-yl)-biphenyl-4-yloxy]-3-phenyl-propionic acid The title compound was prepared from 4′-(2-benzyl-benzofuran-3-yl)-biphenyl-4-ol, and 3-phenyllactic acid methyl ester, in substantially the same manner, as described in Example 1, steps g-h, and was obtained as a white solid, mp 164-166 C.; MS m/e 524 (M+); Analysis for: C36H28O4 Calc’d: C, 82.42; H, 5.38 Found: C, 82.14; H, 5.20.

Statistics shows that 13674-16-3 is playing an increasingly important role. we look forward to future research findings about Methyl 2-hydroxy-3-phenylpropanoate.

Reference:
Patent; American Home Products Corporation; US6232322; (2001); B1;,
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Synthetic Route of 702-98-7, 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 702-98-7, name is 2-Methyladamantan-2-ol. This compound has unique chemical properties. The synthetic route is as follows.

REFERENCE EXAMPLE 1 Synthesis of 2-methyleneadamantane One liter flask equipped with a Dean-Stark condenser was charged with 166.3 g (1.0 mol) of 2-methyl-2-adamantanol (supplied by Sigma-Aldrich Co.), 2.0 g (20 mmol) of sulfuric acid and 500 g of toluene. The content was heated to the solvent reflux temperature. While toluene and water produced through the reaction were collected as an azeotrope by the Dean-Stark condenser, the reaction mixture was refluxed for 2 hours. After completion of the reaction, the catalyst was removed by washing the reaction mixture with water and the obtained organic phase was concentrated to dryness to give 152.5 g of white solid 2-methyleneadamantane (purity: 99.0%, yield: 98.0%).

According to the analysis of related databases, 702-98-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; TOSOH CORPORATION; US2003/139613; (2003); 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. 7287-81-2, name is 1-(m-Tolyl)ethanol. A new synthetic method of this compound is introduced below., Safety of 1-(m-Tolyl)ethanol

General procedure: A 1,2-dichloroethane (2.0 or 5.0 mLmL) solution of alcohol 1 (0.3mmol), enol acetate 2 (0.3mmol), and ReBr(CO)5 (5mol%) was stirred under an atmosphere of nitrogen at 80C for 5h. After the reaction was complete, H2O was added to the reaction mixture and extracted with ethyl acetate. The organic layer was dried with MgSO4. The resulting mixture was filtered, and the filtrate was concentrated. Purification of the residue by silica gel column chromatography afforded carbonyl compounds. Further purification was carried out by recyclable preparative HPLC, if necessary. The structures of the products were assigned by their 1H and 13C NMR, and mass spectra. The product was characterized by comparing its spectral data with those of authentic sample or previous reports 3a [23], 3b [24], 3c [24a], 3e [25], 3f [24a,26], 3h [27], 3i [28], 3j [29], 3k [25], 3l [30], 3m [31], 4b [27], 4d [32], 4g [24a,33], 4h [34], 6a [35], 6g [24a], 6h [36], 8e [37], and 8e? [38]. The structures of the products (3d, 4c, 4e, 4f, 4i, 6b, 6c, 6d, 6e, 6f, 6i, 6j, 6k, 6l, 8a, 8a?, 8b, 8b?, 8c, 8c?, 8d, 8d?, 8f, 8f?, 8g, and 8g?) were assigned by their 1H and 13C NMR, IR, and high resolution mass spectra analysis.

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, 7287-81-2, 1-(m-Tolyl)ethanol.

Reference:
Article; Umeda, Rui; Takahashi, Yuuki; Yamamoto, Takaaki; Iseki, Hideki; Osaka, Issey; Nishiyama, Yutaka; Journal of Organometallic Chemistry; vol. 877; (2018); p. 92 – 101;,
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Reference of 599-67-7, 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.599-67-7, name is 1,1-Diphenylethanol, molecular formula is C14H14O, molecular weight is 198.26, as common compound, the synthetic route is as follows.

General procedure: The procedure is the same for solid and liquid substrates.Alcohol (1 mmol) and iodine (3 mol%) weremixed together in a 5 mL conical reactor and the reactionmixture stirred at 25 C or 55 C for various times (5 minto 192 h), progress was monitored by TLC or by 1H NMRspectroscopy. The crude reaction mixture was dilutedwith tert-butyl methyl ether, washed with an aqueoussolution of Na2S2O3, water, dried over Na2SO4 and the solventevaporated under reduced pressure. The crude reactionmixture was subjected to column chromatography orpreparative TLC using hexane or petroleum ether/tert-butylmethyl ether mixtures and pure product(s) were obtained.Conversions were determined by 1H NMR spectroscopy.The effects of reaction variables on the type oftransformation and conversions are stated in Tables andFigures. In order to obtain the information (role) of thereaction variables and structure of substrate, the data (reactiontimes with lower conversion) are presented in someTables. In the experimental section, the best reaction conditionsare named; 3 mol% of I2 were used, giving thehighest yield.

Statistics shows that 599-67-7 is playing an increasingly important role. we look forward to future research findings about 1,1-Diphenylethanol.

Reference:
Article; Jereb, Marjan; Vra?i?, Dejan; Acta Chimica Slovenica; vol. 64; 4; (2017); p. 747 – 762;,
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Electric Literature of 2077-19-2, 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. 2077-19-2, name is 2-(4-Bromophenyl)propan-2-ol. A new synthetic method of this compound is introduced below.

To a mixture of A-38 (2.80 g, 13.02 mmol) in THF (30 mL) was added NaH (1.04 g, 26.04 mmol, 60% purity) and CH3I (1.62 mL, 26.04 mmol) at 0 C and the mixture was stirred at 25 C for 16 hours. The mixture was quenched with a saturated solution of NH4C1 (50 mL), extracted with EtOAc (100 mL x 2), and the combined organic phase was washed with brine (30 mL), dried over Na2S04, filtered and concentrated to A-39 (2.70 g, 11.78 mmol) as an oil. 1H NMR (400MHz CDC13) _ = 7.47 (d, 2H), 7.29 (d, 2H), 3.07 (s, 3H), 1.51 (s, 6H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2077-19-2, 2-(4-Bromophenyl)propan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; PRAXIS PRECISION MEDICINES, INC.; REDDY, Kiran; MARTINEZ BOTELLA, Gabriel; GRIFFIN, Andrew, Mark; MARRON, Brian, Edward; (364 pag.)WO2018/98499; (2018); A1;,
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Related Products of 5339-85-5 ,Some common heterocyclic compound, 5339-85-5, 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.

Example 49 2-(2-(2-hydroxyethyl)phenyl)isoindoline-1,3-dione; [0379] A flask containing 2-aminophenethyl alcohol (565 mg, 4.12 mmol), phthalic anhydride (641 mg, 4.32 mmol) and acetic acid (4 mL) was heated at 100 C for 1 h. The reaction mixture was poured into water (30 mL) and the solid was filtered off and the solids were washed with water. The crude was purified by flash column chromatography to afford the desired product as white solid (435 mg, 1.63 mmol, 40%). NMR: 1.79 (br s, 1H), 2.78 (t, 2H, J = 6.4 Hz), 3.81 (t, 2H, J = 6.4 Hz), 7.20 (d, 1 H, J = 8 Hz), 7.36-7.41 (m, 1H), 7.46 (d, 2H, J = 4 Hz), 7.79-7.83 (m, 2H), 7.94-7.97 (m, 2H).

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. 5339-85-5, 2-(2-Aminophenyl)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NEWLINK GENETICS; MAUTINO, Mario, R.; KUMAR, Sanjeev; JAIPURI, Firoz; WALDO, Jesse; KESHARWANI, Tanay; ZHANG, Xiaoxia; WO2011/56652; (2011); A1;,
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Application of 3597-91-9, 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 3597-91-9 as follows.

Step 1. Preparation of biphenyl-4-ylmethy. 2,2,2-trichloroethanimidoate (C93). A suspension of biphenyl-4-yimethanol (36.8 g, 200 mmol) in dichloromethane (240 mL) was treated with 50% aqueous potassium hydroxide solution (160 mL). The reaction mixture was cooled to 0″C, and maintained at 0 – 1OC as tetra-rt-butylammonium sulfate (1.18 g, 2,0 mmol) was added, followed by a slow addition of trichtoroacetonitrile (25.1 mL, 250 mmol) over 10 minutes. The reaction was stirred at OC for an hour, and then stirred at 25C for an additional hour, after which the organic layer was filtered through a short pad of Celite on top of a layer of silica gel. The pad was rinsed with additional methylene chloride (1500 mL), and the elubetants were concentrated in vacuo to provide C93 as a white solid, which was used in the next step without purification. Yield: 66.1 g, quantitative. LCMS m/z 167.2 (C13H1 1′). 1H NMR (400 MHz, CDCI3) 6 5.40 (s, 2H), 7,37 (m, 1 H), 7.46 (m, 2H), 7.52 (d, J?8.7 Hz, 2H), 7,62 (m, 4H), 8.43 (br s, 1 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3597-91-9, its application will become more common.

Reference:
Patent; PFIZER INC.; BROWN, Matthew Frank; DONOVAN, Charles Francis; ELLSWORTH, Edmund Lee; HOYER, Denton Wade; JOHNSON, Timothy Allen; LALL, Manjinder Singh; LIMBERAKIS, Chris; MURPHY, Sean Timothy; SHERRY, Debra Ann; TAYLOR, Clarke Bentley; WARMUS, Joseph Scott; WO2010/32147; (2010); A2;,
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