Month: August 2021

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. 349-75-7, name is (3-(Trifluoromethyl)phenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. HPLC of Formula: C8H7F3O

The title compound was prepared from intermediate 6 using the method of example 45 with the reaction being facilitated with microwave irradiation at 120 C. for 20 min: white solid, 20 mg, 16.5% yield: 1H-NMR (DMSO-d6) delta 7.74-7.80 (m, 3H), 7.62-7.66 (m, 1H), 7.37-7.39 (m, 2H), 7.28 (d, 2H), 5.63 (s, 2H), 5.27 (d, 2H), 3.48 (s, 3H), 3.18 (s, 3H). LCMS retention time 2.992 min; LCMS MH+ 479.

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, 349-75-7, (3-(Trifluoromethyl)phenyl)methanol.

Reference:
Patent; HYDRA BIOSCIENCES, INC.; Chenard, Bertrand L.; Gallaschun, Randall J.; Kimball, Spencer David; US2014/275528; (2014); A1;,
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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.2979-22-8, name is 2-Methoxy-2-phenylethanol, molecular formula is C9H12O2, molecular weight is 152.19, as common compound, the synthetic route is as follows.COA of Formula: C9H12O2

General procedure: An aldehyde (30 mmol), Zn(OTf)2 (13 mg, 35 mmol), and (N-Chloroethyl)morpholine HCl 6.5 mg, 35 mmol) were added to a 1dram vial. The dry solvent, acetonitrile (1mL), was added to the vial. Afterwards dipicolylamine (7 muL 35 mmol) was added to the vial and the vial was sonicated. Once the solution was transparent molecular sieves were added to the solution along with the respective alcohol (175 mmol). The assemblies were incubated for 16 h at room temperature in the dark.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2979-22-8, 2-Methoxy-2-phenylethanol, and friends who are interested can also refer to it.

Reference:
Article; Minus, Matthew B.; Featherston, Aaron L.; Choi, Sooyun; King, Sam C.; Miller, Scott J.; Anslyn, Eric V.; Chem; vol. 5; 12; (2019); p. 3196 – 3206;,
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Related Products of 1562-00-1 , The common heterocyclic compound, 1562-00-1, name is Sodium isethionate, molecular formula is C2H5NaO4S, 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 20 g of CH3CN was added 2-hydroxyethanesulfonic acid sodium (27) 4.7 g, 2.9 g of triethylamine, 4-dimethylaminopyridine24 mg were dissolved,(24) obtained in the above (Synthesis Example 1-1-3)Was dissolved in 20 g of CH3CN dropwise at 20 or lower, The mixture was stirred at 25 for 2 hours to obtain a sulfonic acid salt (25). 20 g of CH2Cl2 and 34 g of an aqueous solution of triphenylsulfonium chloride were added, And stirred for 30 minutes. After separating the organic layer,The aqueous layer was extracted with CH2Cl2,The combined organic layers were washed three times with H2O.The solvent was distilled off under reduced pressure,8.4 g of the target compound (PAG-1) was obtained (yield of 57% in three steps).

The synthetic route of 1562-00-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shin-Etsu Chemical Co., Ltd.; Domon, Daisuke; Masnaga, Keiichi; Sakehashi, Masayoshi; Watanabe, Satoshi; (33 pag.)KR2015/71677; (2015); A;,
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Adding a certain compound to certain chemical reactions, such as: 3597-91-9, [1,1′-Biphenyl]-4-ylmethanol, 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: 3597-91-9, blongs to alcohols-buliding-blocks compound. Recommanded Product: 3597-91-9

General procedure: To a Schlenk tube were added Fe(NO3)3·9H2O (40.6 mg, 0.1 mmol), TEMPO (15.8 mg, 0.1 mmol), KCl (7.5 mg, 0.1 mmol), 1a (108.5 mg, 1.0 mmol), and DCE (4.0 mL) sequentially under an atmosphere of oxygen (gas bag, commercial size: 2 L, which could be expanded to 5 L). The mixture was then stirred at 25 C until completion of the reaction as monitored by TLC (petroleum ether/EtOAc = 5:1) (48h). The crude reaction mixture was filtered through a short column of silica gel (height: 2 cm, diameter: 3 cm) eluting with Et2O (3 × 25 mL). After evaporation, the residue was purified by chromatography on silica gel [petroleum ether/EtOAc = 15:1 (500 mL) to 2:1 (300 mL)] to afford benzoic acid (2a)14 (69.9 mg, 57%) as a pale yellow solid. Yields of 57% of 2a and 38% of benzaldehyde (3a)15 were observed by NMR analysisof the crude product using CH2Br2 as an internal standard and by comparison with spectra reported in the literature.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,3597-91-9, [1,1′-Biphenyl]-4-ylmethanol, and friends who are interested can also refer to it.

Reference:
Article; Jiang, Xingguo; Ma, Shengming; Synthesis; vol. 50; 8; (2018); p. 1629 – 1639;,
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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 66102-69-0, name is 3-Amino-2-benzylpropan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. Computed Properties of C10H15NO

Preparation of 3-amino-2-benzyl-1-propanesulfonic acid (Compound N4); To a cold (-78 C.) solution of 3-hydroxypropionitrile (1 g, 14.06 mmol) in THF (30 mL), was added a solution of lithium bis(trimethylsilyl)amide (1 M in THF, 28 mL). After the reaction mixture was stirred for 1 h at -78 C., benzyl bromide (1.67 mL, 14.06 mmol) was added dropwise and the reaction mixture was warmed to reach 0 C. at which temperature the mixture was stirred overnight. The reaction was quenched with 1N HCl and extracted with EtOAc. The organic layer was washed with 1N HCl, dried over Na2SO4 and concentrated. The residue was applied on silica gel column (eluant:Hexanes:EtOAc 70:30 to 50:50) to afford 1.3 g (69%) of the 2-benzyl-3-hydroxypropionitrile. 1H NMR (300 MHz, CDCl3) delta 2.80 (bs, 1H), 2.95 (m, 3H), 3.77 (m, 2H), 7.20-7.35 (m, 5H); 13C NMR (125 MHz, CDCl3) delta 34.71, 37.03, 61.98, 120.78, 127.58, 129.06, 129.25, 136.71. The dialkylated product was isolated in 8.5% yield. To a solution of 2-benzyl-3-hydroxypropionitrile (obtained in step 1, 3 g, 24.75 mmol) in EtOH (60 mL) was added an aqueous solution of NH4OH (30%, 20 mL), followed by Ra-Ni (3 g). The suspension was stirred under atmosphere H2 pressure for 15 hours and then filtered. The filtrate was concentrated under high vacuum; and the residual product (3-1mino-2-benzyl-1-propanol) was used in the next step without purification. A solution of the crude 3-amino-2-benzyl-1-propanol (4.5 g, 27.23 mmol) in anhydrous CHCl3 (24 mL) was saturated with HCl (g), and then SOCl2 (5.2 mL, 71.0 mmol) was added dropwise at reflux. The reaction was maintained under reflux for an additional 2 hours. The reaction was then concentrated to yield a syrupy product. The crude 3-chloro-2-benzyl-1-propylamine thus obtained was used in the next step without further purification. A solution of the crude 3-chloro-2-benzyl-1-propylamine (obtained in step 3) in water (10 mL) was added dropwise to a solution of Na2SO3 (6.8 g, 54.46 mmol) in water (25 mL) under reflux. After the end of the addition, the reaction was stirred at reflux for 1 hour, then cooled down and concentrated under reduced pressure. HCl (conc. 16 mL) were added to dissolve the aminosulfonic acid and precipitate the inorganic salts which were removed by filtration. The filtrate was concentrated; and ethanol was added. The title amino sulfonic acid was precipitated as white solid which was collected by filtration, washed with EtOH and Et2O, then dried under high vacuum to give a white solid (1.87 g, 30% yield over three steps). 1H NMR (500 MHz, D2O) delta 2.52 (m, 1H), 2.8 (m, 2H), 2.94 (m, 2H), 3.08 & 3.18 (ABX, J=13.0 & 7.0 Hz, 2H), 7.25-7.37 (m, 5H). 13C NMR (125 MHz, D2O) delta 35.47, 37.78, 42.67, 52.55, 127.15, 129.09, 129.54, 138.32. ES-MS 228 (M-1).

With the rapid development of chemical substances, we look forward to future research findings about 66102-69-0.

Reference:
Patent; Neurochem (International) Limited; US2006/223855; (2006); A1;,
Alcohol – Wikipedia,
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Reference of 62058-03-1, 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. 62058-03-1, name is trans-4-Aminoadamantan-1-ol. A new synthetic method of this compound is introduced below.

Example B .3 Preparation of compound 3; A mixture of 2-[(p-chlorophenyl)sulfonyl]-2-methylpropionic acid [28361-38-8] (0.00028 mol) in dichloromethane (5 ml) and DMF (5 ml) was stirred and 1-hydroxy- lH-benzotriazole (O.OOO33 mol) was added. Then the mixture was stirred for 10 minutes and iV-(ethylcarbonimidoyl)-iV,iV-dimethyl-l,3-propanediamine, monohydrochloride [25952-53-8] (O.OOO33 mol) was added. The resulting mixture was stirred for 10 minutes and (lalpha,3alpha,4alpha,5beta,7alpha) -4-aminotricyclo[3.3.1.13’7]decan-l-ol [62058-03-1] (O.OOO33 mol) was added. The reaction mixture was stirred overnight at room temperature and then the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2CyCH3OH 98/2). The product fractions were collected and the solvent was evaporated, yielding 0.094 g of compound 3.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,62058-03-1, trans-4-Aminoadamantan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2006/24627; (2006); A2;,
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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. 149965-40-2, name is (5-Bromo-2-chlorophenyl)methanol, the common compound, a new synthetic route is introduced below. Recommanded Product: (5-Bromo-2-chlorophenyl)methanol

[179.1] (5-Bromo-2-chlorophenyl)methanol (8.187 g) was dissolved in 100 ml of toluene, 12.2 g of diphenylposhorazide and 6.52 ml of diazabicycloundecene were added successively, and the mixture was stirred overnight at room temperature. After ethyl acetate was added thereto, the reaction mixture was successively washed with water and brine, dried over anhydrous magnesium sulfate, and the solvent was removed. The residue was purified by silica gel column, to give 9.75 g of the title compound in the 50:1 hexane-ethyl acetate fraction.1H-NMR(CDCl3) delta: 4.48 (s, 2H) 7.28 (d, J=8.4Hz, 1H) 7.41 (dd, J=2.4, 8.4Hz, 1H) 7.56 (d, J=2.4Hz, 1H)

The synthetic route of 149965-40-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Eisai Co., Ltd.; EP1394147; (2004); A1;,
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Application of 34231-22-6, 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. 34231-22-6, name is 3-(Aminomethyl)benzyl Alcohol, molecular formula is C8H11NO, 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.

3-Aminomethylbenzyl alcohol (1.12 g, 8.2 mmol) was weighed into a 100 mL round bottom flask,Tetrahydrofuran (10 mL) was added and triethylamine (0.873 mL, 6.2 mmol) was added to the reaction mixture.Trifluoroacetic anhydride (0.897 mL, 6.2 mmol) was added dropwise under ice-cooling,Dropping process continued for about 30min, dropping to room temperature after stirring the reaction 3.5h,The progress of the reaction was monitored by TLC. After the reaction was completed,Adding ethyl acetate and water according to a volume of 1: 1 composition of the mixture was extracted,After the organic phase was washed with saturated ammonium chloride solution,After drying over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure at 37 C,Purification by silica gel column chromatography, eluent ethyl acetate and petroleum ether,With gradient elution,The volume ratio of ethyl acetate / petroleum ether gradually increased from 1: 1 to 1: 2,Drying in vacuo at 37 C gave 2,2,2-trifluoro-N- (3- (hydroxymethyl) benzyl) acetamide (1.54 g,6.56 mmol) in 80% yield.

According to the analysis of related databases, 34231-22-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Beijing University of Technology; Zhao Lijiao; Liu Junjun; Lai Xinxin; Song Xiuqing; Ren Ting; Zhong Rugang; (29 pag.)CN107235981; (2017); A;,
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Application of 6240-11-5, Adding some certain compound to certain chemical reactions, such as: 6240-11-5, name is 1-Adamantaneethanol,molecular formula is C12H20O, 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 6240-11-5.

Adamantyl acetaldehyde: To a flask containing 2-adamantyl-1-ethanol (5 g, 27.7 mmol) in CH2Cl2 (28 mL) was added TEMPO (433 mg, 2.77 mmol) followed by iodobenzene diacetate (9.8 g, 30.5 mmol). The reaction was stirred 1 hour and then diluted with CH2Cl2 (100 mL). Saturated aqueous solution of Na2S2O3 (100 mL) was added and extracted with CH2Cl2 (3×50 mL). The combined organics were washed with saturated aqueous NaHCO3 (150 mL) and brine (150 mL), dried over Na2SO4, and concentrated in vacuo. The resulting residue was purified by silica gel chromatography (5% Et2O/pentanes) to provide the title compound, which was identical to the reported literature compound (see Luly et al. (1987) J. Org. Chem. 52: 1487).

According to the analysis of related databases, 6240-11-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; California Institute of Technology; US2006/189830; (2006); A1;,
Alcohol – Wikipedia,
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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. 30379-58-9, name is Benzyl 2-hydroxyacetate, the common compound, a new synthetic route is introduced below. Safety of Benzyl 2-hydroxyacetate

To a solution of lithium 3-(cyclopropylmethoxy)-4-(N-(2-(4-methylpiperazin-1-yl)ethyl)methylsulfonamido)benzoate (theoric 0.869 mmol) and EDC (349 mg, 1.821 mmol) in dry DCM (3 ml), benzyl 2-hydroxyacetate (151 mg, 0.910 mmol) and DMAP (111 mg, 0.910 mmol) were added at RT. The final mixture was stirred for 2 days, then the solvent was evaporated, the residue was portioned between water and EtOAc, the organic layer was washed with NaHCO3 sat. sol. and brine, dried over Na2SO4 and evaporated. The crude was purified by flash chromatography on silica gel (eluent: DCM/MeOH/32% NH4OH 95/5/0.5) to give 2-(benzyloxy)-2-oxoethyl 3-(cyclopropylmethoxy)-4-(N-(2-(4-methylpiperazin-1-yl)ethyl)-methylsulfonamido)benzoate as a colorless oil (370 mg, 0.661 mmol, 76% yield over 2 steps, MS/ESI+ 560.1 [MH]+)

The synthetic route of 30379-58-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chiesi Farmaceutici S.p.A.; ARMANI, Elisabetta; Amari, Gabriele; Capaldi, Carmelida; Esposito, Oriana; Peretto, Ilaria; US2013/79313; (2013); A1;,
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