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. 1777-82-8, name is (2,4-Dichlorophenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. COA of Formula: C7H6Cl2O

General procedure: A mixture of 6 mmol of the alcohol or the amine and5 mmol o-phenylenediamine, o-aminophenol or o-aminothiophenol,10 mol % Fe2(SO4)3, 10 mol % TEMPO wasprepared in a 10 ml three-necked flask, and then stirred inopen air at 110 C for several hours, The reaction progresswas monitored by TLC. When the final reaction mixturecooled to room temperature, the crude products was directlypurified by column chromatography on silica gel using hexane/ethyl acetate (7:3) as eluent to afford the pure product.

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, 1777-82-8, (2,4-Dichlorophenyl)methanol.

Reference:
Article; Yu, Jiatao; Shen, Mengnan; Lu, Ming; Journal of the Iranian Chemical Society; vol. 12; 5; (2015); p. 771 – 778;,
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Synthetic Route of 14002-80-3 ,Some common heterocyclic compound, 14002-80-3, molecular formula is C6H12O3, 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.

Compound 42; 3-[4-[1-(1-(2-(1-piperidinyl)phenyl)pentyl)aminocarbonylmethyl]phenoxy]-2,2-dimethylpropanoic acid; This product was synthesized in 3 steps. Step 1; 2-(methoxycarbonyl)-2-methylpropyl 4-methylbenzenesulfonate; Methyl 3-hydroxy-2,2-dimethylpropanoate (5.0 g, 37.83 mmol) was solubilized in dichloromethane (50 ml) and triethylamine (16.0 ml, 113.5 mmol) was added. The mixture was cooled to 0 C. and p-toluenesulfonyl chloride (7.2 g, 37.83 mmol) was added portionwise. The mixture was stirred at room temperature for 4 days and was thenhydrolyzed by water (50 ml). Layers were decanted and the organic phase was washed with 1M HCl (2×50 ml) and NaClsat (2×50 ml). It was dried with magnesium sulfate, filtered and concentrated and the resulting residue was purified by silica gel chromatography (cyclohexane/ethyl acetate 8/2). Yield: 29%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,14002-80-3, its application will become more common.

Reference:
Patent; GENFIT; US2006/79696; (2006); A1;,
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Related Products of 57267-78-4, 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 57267-78-4, name is Ammonium 2-hydroxyethanesulfonate. This compound has unique chemical properties. The synthetic route is as follows.

22 mg of crude oltipraz powder is added into a glass round bottom flask equipped with a magnetic stirrer and cold-water condenser. To the flask was added 10 ml of acetone at room temperature and 30 mg of isethionic acid ammonium salt is slowly added into the solution while stirring is continued. Once all the isethionic acid ammonium salt has been added, the temperature is increased and set to reflux for 6 hrs. Released ammonia is captured in a dilute hydrochloric acid trap from the top of the condenser. After 6 hrs the reaction is brought to pH 6.8 with minimum quantity of concentrated hydrochloric acid and the resultant mixture is evaporated, under vacuum, to dryness to yield the isethionic acid complex of oltipraz as a red/brown solid. FTIR: C=S peaks 1216/1228 (relative intensity 9: 1) and 464/435 (relative intensity 9: 1).

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 57267-78-4, Ammonium 2-hydroxyethanesulfonate.

Reference:
Patent; ST IP HOLDING AG; FRAMROZE, Bomi; (0 pag.)WO2020/58767; (2020); A1;,
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Reference of 2240-88-2, Adding some certain compound to certain chemical reactions, such as: 2240-88-2, name is 3,3,3-Trifluoropropan-1-ol,molecular formula is C3H5F3O, 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 2240-88-2.

(S)-tert-Butyl2-((5-fluoro-4-hydroxy-2-methoxybenzyl)carbamoyl)pyrrolidine-1-carboxylate ( 400 mg, 1.086 mmol, see example 1 ), triphenylphosphine (575 mg, 2.172mmol) and 3,3,3-trifluoropropan-1-ol (0.144 mL, 1.629 mmol) were dissolved in THF (12 mL) under inert atmosphere. The reaction mixture was cooled to -10°C and DIAD(0.444 mL, 2.172 mmol) was added dropwise via syringe and stirring at -1 0°C continuedfor 2h. Subsequently the cooling bath was removed and the reaction mixture stirredat room temperature over the weekend. Since the reaction was not complete, additionaltriphenylphosphine (575 mg, 2.172 mmol), 3,3,3-trifluoropropan-1-ol (0.144 mL, 1.629 mmol) and DIAD (0.444 mL, 2.172 mmol) were added to the reaction mixture at -5°Cand the reaction stirred at room temperature overnight. Since the reaction was still incomplete,once again DIAD (0.444 mL, 2.172 mmol) was added at -5°C and the reaction stirred at room temperature overnight. Water was added, the reaction mixture extractedthree times with ethyl acetate, the organic phases were combined and dried oversodium sulfate. Evaporation of the solvent and purification of the raw material by columnchromatography resulted in (S)-tert-butyl 2-((5-fluoro-2-methoxy-4-(3,3,3-trifluoropropoxy)benzyl)carbamoyl)pyrrolidine-1-carboxylate (180 mg; yield 37percent)BOC deprotection and subsequent salt formation was performed as described in example1 resulting in (2S)-N-[[5-fluoro-2-methoxy-4-(3,3,3-trifluoropropoxy)phenyl]methyl]pyrrolidine-2-carboxamide fumarate as white powder after lyophilization.LC-MS (M/Z [M+Ht): 365.2 1HNMR (500 MHz, methanol-d4) 8 7.03 (d, J= 11.5 Hz, 1H), 6.74 (d, J= 7.0 Hz, 1H),6.68 (s, 2H), 4.36, 4.31 (ABq, J = 14.8 Hz, 2H), 4.30 (t, J = 6.1 Hz, 2H), 4.23 (dd, J =8.4, 6.8 Hz, 1H), 3.85 (s, 3H), 3.39 (dt, J = 11.4, 7.0 Hz, 1H), 3.35- 3.27 (m, 1H), 2.76-2.63 (m, 2H), 2.45-2.34 (m, 1H), 2.08- 1.92 (m, 3H).

According to the analysis of related databases, 2240-88-2, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ABBVIE DEUTSCHLAND GMBH & CO. KG; ABBVIE INC.; BACKFISCH, Gisela; BAKKER, Margaretha; BLACK, Lawrence; BRAJE, Wilfried; DRESCHER, Karla; ERHARD, Thomas; HAUPT, Andreas; HOFT, Carolin; KLING, Andreas; LAKIS, Viktor; MACK, Helmut; RELO, Ana Lucia; (111 pag.)WO2018/175449; (2018); A1;,
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Reference of 10029-04-6 ,Some common heterocyclic compound, 10029-04-6, molecular formula is C6H10O3, 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.

1.0 g (7.7 mmol) hydroxymethyl acrylate was dissolved in 1.5 mol 5 weight-% sodium hydroxide solution (0.46 g; 11.6 mmol NaOH) and stirred for 4 hours at room temperature. After several extractions with diethyl ether, the ether phase was washed with water, dried over calcium chloride and the product was dried in vacuum. Yield: 0.47 g (60%) 1H-NMR [ppm]: delta (500 MHz, CDCl3)=3.2 (HO-CH2); 4.2 (HO-CH2); 5.85 (=CH2); 6.25 (=CH2); 12.5 (O=C-OH)

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. 10029-04-6, Ethyl 2-(hydroxymethyl)acrylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; DENTSPLY International Inc.; KLEE, JOACHIM E; RITTER, HELMUT; POHLE, SVEN; ELSNER, OLIVER; BARDTS, MAREIKE; US2015/238390; (2015); A1;,
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Related Products of 1805-32-9, 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 1805-32-9, name is 3,4-Dichlorobenzyl alcohol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The oxidation of alcohols was performed in an autoclave reactor equipped with a magnetic stirrer, thermocouple, automatic temperature controller and a pressure gauge. After the addition of desired amount of reactant, catalyst, water and NaOH, the autoclave was sealed. The atmosphere over the mixture was replaced with O2 for three times. Then the reactor was heated to the desired temperature with stirring. Subsequently, the pressure of O2 was charged to 1.0 MPa and kept constant during the reaction through feeding O2. When the reaction was finished, the reactor was cooled down to the ambient temperature. The reaction mixture was diluted with acetone to dissolve the products. After the catalyst was separated, the filtrate was acidified to pH of 2.0 by hydrochloric acid. The oxidation products were analyzed by gas chromatography equipped with a flame ionization detector. The isolated yield of carboxyl acid was obtained with the following procedure. The solvent of the mixture after acidification was removed through rotary evaporation. The pH of the residual was adjusted to 10.0 with NaOH (2.0 M), and then it was extracted with ethyl acetate for three times. The aqueous layer was acidified to pH 2.0 using HCl (6.0 M) and extracted with ethyl acetate. The organic layer was removed ethyl acetate through rotary evaporation to get the carboxylic acid. The carboxylic acid was dried overnight for calculation of the isolated yield.

According to the analysis of related databases, 1805-32-9, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhou, Lipeng; Chen, Minzhu; Wang, Youqiang; Su, Yunlai; Yang, Xiaomei; Chen, Chen; Xu, Jie; Applied Catalysis A: General; vol. 475; (2014); p. 347 – 354;,
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Related Products of 34231-22-6, 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.34231-22-6, name is 3-(Aminomethyl)benzyl Alcohol, molecular formula is C8H11NO, molecular weight is 137.18, as common compound, the synthetic route is as follows.

Fmoc-OSu (38.6 g, 115 mmol) was added to a solution of [3-(amino-methyl)phenyl]methanol (S14, 16.5 g, 121 mmol) in THF (150 mL), water (75 mL) and sodium bicarbonate (20.3 g, 241 mmol) at room temperature (rt) and the reaction stirred overnight (o/n). At that point, a small sample was diluted with MeOH, acidified with a drop of HOAc, and analyzed by LC-MS, which showed the desired product with no Fmoc-OSu reagent. The reaction was acidified with 1M HCl, diluted with ethyl acetate (EtOAc), and stirred for 2 h. The white solid was filtered off, washed well with water, then EtOAc, and air dried for 3 h until a constant weight was attained. The product thus obtained, Fmoc-S14 (15.3 g), was found by LC-MS to be free of identifiable organic impurities. The aqueous layer was extracted with EtOAc (2×). The combined organic layers were washed with H2O (2×) and brine, then dried over anhydrous MgSO4. The desiccant was removed by filtration and the filtrate concentrated under reduced pressure to give additional amounts of the desired product as a white solid (34.1 g). The combined solids were triturated with ethyl acetate at reflux for a few minutes, then o/n at rt to give Fmoc-S14 in 88% yield (38.1 g).

Statistics shows that 34231-22-6 is playing an increasingly important role. we look forward to future research findings about 3-(Aminomethyl)benzyl Alcohol.

Reference:
Patent; CYCLENIUM PHARMA INC.; MACDONALD, Dwight; DUBE, Daniel; WAHHAB, Amal; THOMAS, Helmut; RICHARD, Luc; PETERSON, Mark L.; US2019/153620; (2019); A1;,
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Synthetic Route of 748805-85-8, 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 748805-85-8 as follows.

General procedure: Benzyl alcohol derivative 11 (1 eq.) was dissolved in CH2Cl2 (0.4 M). Manganese (IV) oxide (2.1 eq.)was added under argon and the solution was left to stir at room temperature for 48 h. The progress ofthe reaction was monitored by TLC analysis. After completion, manganese oxide was filtered off andthe resulting filtrate was concentrated under reduced pressure. The crude product was purified by silicacolumn chromatography employing mixtures of n-hexane and ethyl acetate as eluents to obtain thedesired product 10.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,748805-85-8, its application will become more common.

Reference:
Article; Jarrige, Lucie; Merad, Jeremy; Zaied, Siwar; Blanchard, Florent; Masson, Geraldine; Synlett; vol. 28; 14; (2017); p. 1724 – 1728;,
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Electric Literature of 80466-51-9 ,Some common heterocyclic compound, 80466-51-9, molecular formula is C11H17NO, 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: The solution of boronic acid 4 (9.4 mg, 0.025 mmol, 5 mol%) and aminoalcohol (5.2 mg, 0.025 mmol, 5 mol%) was refluxed in toluene for12 h to remove water azeotropically. The mixture was allowed to coolto r.t. and toluene was removed in vacuo. Next, 1 M SnCl4 in CH2Cl2(25 muL, 0.025 mmol, 5 mol%) was added to a solution of the oxazaborolidine,methacrolein (43 muL, 0.5 mmol, 1 equiv), and cyclopentadiene(125 muL, 1.5 mmol, 3 equiv) in CH2Cl2 (2.5 mL) and the mixturewas stirred for 2 h at -78 C. The reaction was quenched with sat. aqNaHCO3 and extracted with Et2O. The combined organic phase waswashed with brine, and dried (Na2SO4). After filtration and removal ofsolvent, the crude product was purified by column chromatography(silica gel, pentane/Et2O 9:1) to afford the Diels-Alder adduct (67 mg,98%) as a colorless oil. The enantioselectivity was determined to be84% ee by GC analysis after conversion into the chiral acetal by(2R,4R)-pentane-2,4-diol.GC [ULBON HR-20M (PEG-20M), 100 C]: tR = 24.3 (minor), 26.0 min(major).1H NMR (400 MHz, CDCl3): delta = 9.70 (s, 1 H), 6.31 (dd, J = 2.9, 6.1 Hz, 1H), 6.11 (dd, J = 6.1, 3.0 Hz, 1 H), 2.87 (br s, 1 H), 2.81 (br s, 1 H), 2.22(dd, J = 3.8, 12.0 Hz, 1 H), 1.35-1.42 (m, 1 H), 1.22-1.28 (m, 1 H), 1.00(s, 3 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,80466-51-9, its application will become more common.

Reference:
Article; Shimoda, Yasushi; Yamamoto, Hisashi; Synthesis; vol. 49; 1; (2017); p. 175 – 180;,
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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. 217479-60-2, name is 2,4,6-Trichlorobenzyl alcohol, the common compound, a new synthetic route is introduced below. Recommanded Product: 217479-60-2

a) Preparation of 1 ,3,5-trichloro-2-chloromethyl-benzene:To a stirred solution of 2,4,6-trichlorobenzylalcohol (10.0g; 47.3 mmoles) in chloroform (100ml) kept under nitrogen atmosphere, thionyl chloride (6.07ml_, 85.1 mmole) was added slowly at O0C over a period of 15 minutes followed by catalytic amount of DMF The reaction mix was allowed to stir at ambient temp for 3 hours. The reaction mixture was quenched with 5OmL of water; the aqueous layer was extracted with DCM (3 X 100ml). The combined organic layer was washed with 5% sodium bicarbonate solution (2 x 50ml) followed by brine (50ml) and dried over anhydrous sodium sulphate. The solvent was evaporated under reduced pressure. 10.9g (100.0% of theory) of 1 ,3,5-trichloro-2-chloromethyl-benzene was obtained in form of a white solid.1 HNMR (CDCI3, 400MHz): delta= 7.37 (2H, s); 4.82 (2H, s) Mass: M = 229.8

The synthetic route of 217479-60-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; RAJAN, Ramya; WALTER, Harald; STIERLI, Daniel; WO2010/63700; (2010); A2;,
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