Month: March 2022

Application of 144284-25-3, Adding some certain compound to certain chemical reactions, such as: 144284-25-3, name is 2,4,5-Trifluorobenzyl alcohol,molecular formula is C7H5F3O, 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 144284-25-3.

To 25mL sealed tube were added norcantharidin 4 (1.0mmol, 168mg), 4-DMAP (1.0mmol, 244mg), after argon replacement three times, then added DCM 2.5mL, 2,4,5-trifluoro Benzyl alcohol 5 (2.0mmol, 232muL) was reacted at 60 for 14h. After the reaction was completed, it was cooled to room temperature, washed three times with HCl (1 mol/L) and saturated brine, and the organic phases were combined. After the organic phases were dried over anhydrous sodium sulfate, flash column chromatography gave a white solid product 6-3, yield 37.9%.

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. 144284-25-3, 2,4,5-Trifluorobenzyl alcohol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Zunyi Medical University; Jia Jia; He Chunyang; Zhu Erlin; Wang Le; Li Xiaofei; Zhang Jianyong; (9 pag.)CN111253415; (2020); A;,
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Related Products of 72995-94-9, 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. 72995-94-9, name is 14-Bromotetradecan-1-ol, molecular formula is C14H29BrO, 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.

A mixture of 14-bromotetradecan-1-ol (700 mg, 2.38 mmol) and DAST (0.63 ml_, 4.76 mmol) was heated at 35 C for 4h. The reaction mixture was poured into water and extracted with DCM (x3). The combined organic extracts were washed with brine, dried over magnesium sulfate, filtered and the solvent was removed under reduced pressure. The residue was purified by flash chromatography (hexanes/diethyl ether) to yield the title compound (422 mg, 60%) as a colourless oil. 1 H NMR d (400 MHz, CDCI3): 1.21-1.34 (m, 16H), 1.35-1.47 (m, 4H), 1.60-1 .78 (m, 2H), 1.80-1 .92 (m, 2H), 3.41 (t, J=6.9 Hz, 2H), 4.38 (t, J=6.2 Hz, 1 H), 4.50 (t, J=6.2 Hz, 1 H).

According to the analysis of related databases, 72995-94-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ALMIRALL, S.A.; BACH TANA, Jordi; ESTEVE TRIAS, Cristina; MIR CEPEDA, Marta; (187 pag.)WO2019/115405; (2019); A1;,
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Reference of 1875-89-4, Adding some certain compound to certain chemical reactions, such as: 1875-89-4, name is 2-(m-Tolyl)ethanol,molecular formula is C9H12O, 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 1875-89-4.

General procedure: The alcohol (1.0 eq) was added to a suspension of Dess-Martin periodinane (1.2 eq) in CH2Cl2(100 mM) under an argon atmosphere at room temperature. The mixture was allowed to stir for0.5 – 20 hours, while consumption of starting material was monitored by TLC. After the reactionwas complete, 1M Na2S2O3 (equal volume to CH2Cl2) was added. After stirring for 15 minutes,the phases were separated and the aqueous phase was extracted with CH2Cl2 twice. Thecombined organic layers were washed with 5% NaHCO3 and brine, and dried over Na2SO4. Thesolvent was evaporated under reduced pressure and the residue was purified by columnchromatography to afford analytically pure aldehydes.b) alcohol precursors for aldehydes 13, 14, 20 (solid alcohols)The alcohol (1.0 eq) was dissolved in CH2Cl2 (200 mM) and the solution was added to asuspension of Dess-Martin periodinane (1.2 eq) in CH2Cl2 (200 mM) under an argon atmosphereat room temperature. The mixture was allowed to stir for 0.5 – 20 hours (TLC monitoring). Then,Et2O (equal volume to CH2Cl2), 1M Na2S2O3 and saturated NaHCO3 (both equal volume toCH2Cl2) were added. After stirring for 15 minutes, the phases were separated and the aqueousphase was extracted with Et2O twice. The combined organic layers were washed with sat.NaHCO3 and brine, and dried over Na2SO4. The solvent was evaporated under reduced pressureand the residue was purified by column chromatography to afford analytically pure aldehydes.

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. 1875-89-4, 2-(m-Tolyl)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Ruff, Bettina M.; Bra?se; O’Connor, Sarah E.; Tetrahedron Letters; vol. 53; 9; (2012); p. 1071 – 1074;,
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Adding a certain compound to certain chemical reactions, such as: 18684-63-4, Bicyclo[2.2.2]octan-2-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, SDS of cas: 18684-63-4, blongs to alcohols-buliding-blocks compound. SDS of cas: 18684-63-4

3-(bicyclo-[2.2.2]oct-2-yloxy)-4-Methoxybenzaldehyde Bicyclo[2.2.2]-2-octanol (5.00 g, 40 mmol), isovanillin (6.09 g, 40 mmol) and triphenylphosphine (13.1 g, 50 mmol) are dissolved in dry tetrahydrofuran. To this reaction mixture is added dropwise diethylazodicarboxylate (8.71 g, 50 mmol). The reaction is stirred for 1 hour at room temperature and is refluxed for 80 hours. The reaction mixture was cooled and concentrated in vacuo and the residue is mashed 3*150 ml of ether to remove the desired material from the triphenylphosphine oxide. The combined ethereal layers are washed with 2*100 ml H2 O, 2*100 ml 2N NaOH solution, 2*100 ml H2 O and 2*100 ml brine. The organics are dried, filtered and concentrated in vacuo. The compound is purified by flash silica gel (32-80 mesh) chromatography with 20% ethyl acetate/hexane. The appropriate fractions are concentrated in vacuo to yield 3.32 g (32%) of product as a viscous oil. 1 H NMR (250 MHz, CDCl3): delta 7.4 (dd, 1H, J=8.5 Hz, J=1.5 Hz), 7.35 (d, 1H, J=1.5 Hz), 6.95 (d, 1H, J=8.5 Hz), 4.52 (m, 1H), 3.91 (s, 3H), 2.2-1.3 (m, 12H). 13 C NMR (63 MHz, CDCl3): delta 190.9, 155.7, 147.9, 129.97, 126.2, 112.6, 110.9, 77.5, 56.1, 34.74, 28.18, 25.25, 24.55, 23.29, 22.78, 19.09 (16 lines).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,18684-63-4, Bicyclo[2.2.2]octan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; Pfizer Inc.; US5128358; (1992); A;,
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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. 79944-63-1, name is (3-Amino-5-chlorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 79944-63-1

Example A24; a) Preparation of intermediate 83; [Show Image] 3-Amino-5-chloro-benzenemethanol (0.0194 mol) was added in one portion to a solution of intermediate 77 (0.0162 mol) in 1,4-dioxane (80 ml). DIPEA (0.0194 mol) was added. The resultant reaction mixture was stirred for 8 hours at room temperature. CH2Cl2 (50 ml) and brine (50 ml) were added. The layers were separated. The organic layer was washed with brine (2 x 20 ml). The organic layers were combined, dried (MgSO4), filtered and the solvent was evaporated, yielding 6 g (90%) of intermediate 83.

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, 79944-63-1, (3-Amino-5-chlorophenyl)methanol.

Reference:
Patent; Janssen Pharmaceutica NV; EP1904461; (2008); A2;,
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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 59012-91-8, name is 4-(Hydroxymethyl)phenyl pivalate. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 59012-91-8

Preparation of 5: A 100 G reactor containing the solution of compound 4 is charged with N-methylpyrrolidine (9.5 kg; 2.0 eq dissolved in 23 kg of dichloromethane). After 10 minutes, compound 4a (14.0 kg; 1.2 eq) is added, followed by 1,8-diazabicyclo[5.4.0]undec-7-ene (10.2 kg; 1.2 eq in 23 kg dichloromethane). The batch is warmed to 20 C. Upon reaction completion (1-9 hours), the solution is diluted with 327 kg of dichloromethane and charged to a 200 G reactor containing pH 4.5 phosphate buffer (334 kg of 1 M KH2PO4). The batch is agitated for 30 minutes, and the layers are separated. The lower organic layer is washed once more with pH 4.5 phosphate buffer (111 kg of 1 M KH2PO4), then once with brine (212 kg of 2.5% NaCl/water (w:w)). The resulting organic solution is distilled at <35 C. until Karl Fischer analysis of the batch shows <0.05% water. This solution is used directly in the preparation of compound 1f. With the rapid development of chemical substances, we look forward to future research findings about 59012-91-8. Reference:
Patent; AVI BIOPHARMA, INC.; US2009/131624; (2009); A1;,
Alcohol – Wikipedia,
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Reference of 1013031-65-6, 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.1013031-65-6, name is (2,6-Dibromophenyl)methanol, molecular formula is C7H6Br2O, molecular weight is 265.93, as common compound, the synthetic route is as follows.

To a solution of (2,6-dibromophenyl)methanol i-Sa (9.6 g, 36.1 mmol) in DMF (100 mL) at 0 C was added NaH (60%, 2.2 g, 54 mmol) portionwise. The mixture was kept stirring at room temperature for additional 30 mins, followed by the additional of PMBC1 (8.8 g, 54 mmol). The mixture was stirred at room temperature for 2 h, quenched with sat NH4C1, and extracted with EtOAc. The combined organics were washed with brine, dried over Na2504, andconcentrated. The crude residue was purified by flash chromatography (0-10% EtOAc/hexanes)to give the title compound. ?H NMR (400 MHz, CDC13) oe 7.54 (d, J 7.9 Hz, 1H), 7.35 (d, J8.4 Hz, 1H), 7.01 (t, J= 7.9 Hz, 1H), 6.89 (d, J= 8.4 Hz, 2H), 4.81 (s, 2H), 4.58 (s, 2H), 3.81(s, 3H).

The chemical industry reduces the impact on the environment during synthesis 1013031-65-6, I believe this compound will play a more active role in future production and life.

Reference:
Patent; MERCK SHARP & DOHME CORP.; ZHANG, Hongjun; BARR, Kenneth, Jay; LAPOINTE, Blair, T.; GUNAYDIN, Hakan; LIU, Kun; TROTTER, B., Wesley; (67 pag.)WO2017/75185; (2017); A1;,
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Synthetic Route of 431-23-2 ,Some common heterocyclic compound, 431-23-2, molecular formula is C4H7F3O, 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 solution of 3,3,3-trifluoro-2-methylpropan-1-ol (800 mg, 6.25 mmol) in DCM (20mL) was added triethylamine (950 mg, 9.39 mmol). The mixture was cooled to -20 oc andtrifluoromethanesulfonic anhydride (2.20 g, 7.70 mmol) was added. The mixture was stirred at0 oc overnight. The mixture was diluted with DCM (50 mL), washed with 1 M HCl aqueoussolution (50 mLx 2). The separated organic layer was dried over anhydrous Na2S04, and thenconcentrated in vacuo to give the title compound as yellow oil (1.1 g, yield 68% ).1HNMR (400 MHz, CDCh) 8 (ppm): 4.64-4.46 (m, 2H), 2.79-2.67 (m, 1H), 1.29 (d, J= 7.1 Hz,3H).19F NMR (376 MHz, CDCh) 8 (ppm): -71.6, -74.5.

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. 431-23-2, 3,3,3-Trifluoro-2-methylpropan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; CALITOR SCIENCES, LLC; DAI, Weilong; XI, Ning; LI, Minxiong; ZHANG, Tao; LI, Xiaobo; HU, Haiyang; CHEN, Wuhong; WANG, Tingjin; LIU, Jun; (188 pag.)WO2017/48675; (2017); A1;,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 155310-11-5, name is 3-Amino-2,2-difluoropropan-1-ol, the common compound, a new synthetic route is introduced below. HPLC of Formula: C3H7F2NO

To a solution of 3-amino-2,2-difluoro-propan-1-ol (2.00 g, 18.0 mmol, CAS155310-11-5) in a mixed solvents of THF (75 mL) and H2O (75 mL) was added Boc2O (3.93 g, 18.0 mmol) slowly at 0 C. The reaction mixture was stirred at 25 C. for 16 hours. On completion, the reaction mixture was diluted with 1.0 M aq.HCl (100 mL) and extracted with EA (2×150 mL). The combined organic phase was washed with brine (50 mL), dried over Na2SO4, filtered and concentrated in vacuo to give the title compound (3.76 g, 98% yield) as white solid. 1H NMR (400 MHz, CDCl3) delta 5.04 (s, 1H), 4.10-3.87 (m, 1H), 3.76-3.63 (m, 2H), 3.60-3.54 (m, 2H), 1.48 (s, 9H).

The synthetic route of 155310-11-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kymera Therapeutics, Inc.; Mainolfi, Nello; Ji, Nan; Kluge, Arthur F.; Weiss, Matthew M.; Zhang, Yi; (1443 pag.)US2019/192668; (2019); A1;,
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Reference of 81156-68-5, 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.81156-68-5, name is 2,4-Dichlorophenethyl alcohol, molecular formula is C8H8Cl2O, molecular weight is 191.06, as common compound, the synthetic route is as follows.

Example 4 Preparation of methyl 2- [3- (2- (2, 4-dichlorophenyl) ETHOXY) PHENYL- THIOJISOBUTYRATE (ST2534) The title product was prepared according to the procedure described in Method B starting from methyl 2- (3- hydroxyphenylthio) iso-butyrate (prepared as described in example 1) (0.280 g, 1.24 mmol) and DIAD (0.325 g, 1.61 mmol) dissolved in 3 mL of anhydrous THF and added dropwise to a solution of 2,4- dichlorophenetylalcohol (0.260 G, 1.36 mmol), and triphenylphosphine (0.422 g, 1.61 mmol) in 4 mL of anhydrous THF at 0C. The reaction was left overnight under magnetic stirring at room temperature. After this period, the solvent was evaporated and the residue purified by silica gel chromatography using hexane/AcOEt 9.6/0. 4 as eluent. 0.327 g of oily product were obtained (yield: 66 %); TLC: silica gel, eluent hexane/AcOEt 9/1, Fr: 0.34 ; IH NMR (CDC13, 300 MHz) B : 7.40 (d, 1H), 7.20 (m, 3H), 7.00 (m, 2H), 6.90 (dd, 1H), 4.15 (t, 2H), 3.65 (s, 3H), 3.20 (t, 2H), 1.45 (s, 6H); HPLC: Column: Inertisil ODS-3 (5 ZM) 4.6 x 250 mm, T: room temperature, mobile phase CH3CN/H20 90/10 (v/v), pH: as is, flow rate: 0.8 mL/min, 205 nm UV detector, retention time 12.40 min; KF: 0.2 % H20; E. A. conforming for CL9H20CL203S.

The chemical industry reduces the impact on the environment during synthesis 81156-68-5, I believe this compound will play a more active role in future production and life.

Reference:
Patent; SIGMA-TAU INDUSTRIE FARMACEUTICHE RIUNITE S.p.A.; WO2004/56355; (2004); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts