Tag: M.W=0-100

Adding a certain compound to certain chemical reactions, such as: 109-83-1, 2-(Methylamino)ethanol, 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, blongs to alcohols-buliding-blocks compound. Safety of 2-(Methylamino)ethanol

Example 1 N-(2-hydroxy-ethyl)-4-methoxy-2.6,N-trimethyl-benzenesulphonamide (C) [0152] 3,5-dimethylanisol (A) were dissolved in 50.0 L dichloromethane. After cooling to -35 C. a solution of 17.46 kg (149.85 mol) chlorosulphonic acid in 15.0 L dichloromethane was metered in and the mixture was stirred for about another 30 minutes at -35 C.±5 C. After the reaction was complete 40.0 L of water were metered in at -35 C. to 5 C. and then the organic phase was separated off. The organic phase was diluted with 10.0 L dichloromethane, before a solution of 1.23 kg (14.69 mol) of sodium hydrogen carbonate in 29.0 L water was added. After separation of the organic phase and dilution with 10 L of dichloromethane, a solution consisting of 11.58 kg (154.20 mol) of N-methylaminoethanol (B) in 20.0 L dichloromethane was slowly metered in at 10±5 C. After the reaction was complete, a mixture of 42.0 L water and 4.10 kg (42.59 mol) conc. hydrochloric acid was added, starting at 10 C. The organic phase was separated off, diluted with 10.0 L of dichloromethane and the product ( C) was totally freed from the solvent in vacuo. [0154] Yield: 14.34 kg (71% of theory)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,109-83-1, its application will become more common.

Reference:
Patent; Boehringer Ingelheim International GmbH; Pachur, Thorsten; Pfrengle, Waldemar; Birk, Manfred; Schnaubelt, Juergen; Werthmann, Ulrike; US2013/289049; (2013); A1;,
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Reference of 627-30-5, Adding some certain compound to certain chemical reactions, such as: 627-30-5, name is 3-Chloropropan-1-ol,molecular formula is C3H7ClO, 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 627-30-5.

Triphenylphosphine (2.6 g, 10.1 mmol) and 3-chloropropanol (0.69 ml, 8.2 mmol) were added to a suspension of 4-chloro-7-hydroxy-6-methoxyquinazoline (1.65 g, 7. 8 mmol) in dichloromethane (100 ml) under argon. The flask was placed in a water bath at 20 C and di-tert-butyl azodicarboxylate (2.30 g, 10.1 mmol) added portion wise over a few minutes. The reaction mixture was stirred at ambient temperature for 2 hours before solvent evaporation in vacuo. Purification by flash chromatography on silica gel, eluting with ethyl acetate: petroleum ether (3: 7) yielded 4-CHLORO-7- (3-CHLOROPROPOXY)-6-METHOXYQUINAZOLINE (2.0 g, 91 % yield): H-NMR (DMSO d6) : 8.90 (s, 1H), 7.55 (s, 1H), 7.45 (s, 1H), 4.42 (m, 2H), 4.05 (s, 3H), 3.80 (m, 2H), 2.31 (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. 627-30-5, 3-Chloropropan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/113324; (2004); 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.14320-38-8, name is Cyclopent-3-enol, molecular formula is C5H8O, molecular weight is 84.12, as common compound, the synthetic route is as follows.SDS of cas: 14320-38-8

(1) By using 2.2 g of 3-cyclopentenol prepared according to the method described in J. Org. Chem., 25, 26-29 (1960) and 9.2 g of t-butyldiphenylsilyl chloride and by the same procedures as in (1) of the intermediate preparation example 1, there was obtained 8.15 g of 3-cyclopenten-1-yl (t-butyldiphenylsilyl) ether. Yield 97%

At the same time, in my other blogs, there are other synthetic methods of this type of compound,14320-38-8, Cyclopent-3-enol, and friends who are interested can also refer to it.

Reference:
Patent; Sumitomo Chemical Company, Limited; US5925676; (1999); A;,
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Related Products of 616-29-5, 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.616-29-5, name is 1,3-Diaminopropan-2-ol, molecular formula is C3H10N2O, molecular weight is 90.12, as common compound, the synthetic route is as follows.

General procedure: Three di-Schiff base ligands, H2L1, H2L2 and H2L3 weresynthesized in our laboratory by standard methods [10b].Salicylaldehyde (1.05 mL, 10 mM) was mixed with respectivediammines viz. 1,3-diaminopentane (0.596 mL, 5 mM), 1,3-propanediamine (0.42 mL, 5 mM), 1,3-diaminopropan-2-ol(0.295 g, 5 mM) in methanol (20 mL) and the resulting mixtureswere refluxed for ca. 1.5 h and allowed to cool to roomtemperature. The desired yellow crystalline ligands were filteredoff from each solution, washed with methanol, and dried in avacuum desiccator containing anhydrous CaCl2.

Statistics shows that 616-29-5 is playing an increasingly important role. we look forward to future research findings about 1,3-Diaminopropan-2-ol.

Reference:
Article; Seth, Piya; Figuerola, Albert; Jover, Jesus; Ruiz, Eliseo; Ghosh, Ashutosh; Polyhedron; vol. 117; (2016); p. 57 – 63;,
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Application of 2919-23-5, 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. 2919-23-5, name is Cyclobutanol, molecular formula is C4H8O, 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. 2-Cyclobutoxy-5-nitro-pyridine A mixture of 2-chloro-5-nitropyridine (7.12 g, 45.0 mmol) and cyclobutanol (3.40 g, 47.2 mmol) in THF (30 mL) was vigorously stirred at 0 C. while NaH (1.18 g, 46.7 mmol) was added in three portions over ~10-20 s under air (Caution: Extensive gas evolution). Reaction residue was rinsed down with additional THF (5 mL), followed by stirring under positive argon pressure in the ice bath for 1-2 more minutes. The ice bath was then removed and the brown homogeneous solution was stirred for 1 h. The reaction mixture was concentrated under reduced pressure at 80 C., taken up in 0.75 M EDTA (tetrasodium salt) (150 mL), and extracted with CH2Cl2 (1*100 mL, 1*50 mL). The combined organic layers were dried (Na2SO4), concentrated, taken up in MeOH (2*100 mL) and concentrated under reduced pressure at 60 C. to provide the title compound as a thick dark amber oil that crystallized upon standing (7.01 g, 80%). 1H NMR (CDCl3) delta 9.04 (dd, J=2.84 and 0.40 Hz, 1H), 8.33 (dd, J=9.11 and 2.85 Hz, 1H), 6.77 (dd, J=9.11 and 0.50 Hz, 1H), 5.28 (m, 1H), 2.48 (m, 2H), 2.17 (m, 2H), 1.87 (m, 1H), 1.72 (m, 1H).

According to the analysis of related databases, 2919-23-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Gaul, Michael David; Xu, Guozhang; Baumann, Christian Andrew; US2006/281764; (2006); 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.33420-52-9, name is 2,2-Difluoropropan-1-ol, molecular formula is C3H6F2O, molecular weight is 96.076, as common compound, the synthetic route is as follows.Recommanded Product: 33420-52-9

Step 4 (ME-54):A solution of crude ME-53 (3.8 g, 39.58 mmol) in Dimethyl formamide (5 mL) was added to asuspension of sodium hydride (60%; 1 .3 g, 32.5 mmol) in dry dimethyl formamide (20 mL) at 0C and the mixture was stirred at room temperature for 1 h. The reaction mass was again cooled to 0C and a solution of 5-bromo-2-fluoro benzonitrile (2.36 g, 11.8 mmol) in dimethyl formamide (5 mL) was added. The reaction mass was warmed to room temperature and stirred for 30 mm, quenched with saturated ammonium chloride solution and extracted withdiethyl ether. The combined organic layer was washed successively with water, brine; dried over anhydrous sodium sulfate and concentrated in vacuum to afford the crude intermediate. Purification by column chromatography over silica gel (60-l20mesh) and using 8% ethyl acetate in pet ether as the eluent afforded 2.5 g (69.4%) of ME-S4 as a yellow gummy liquid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,33420-52-9, 2,2-Difluoropropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; PROBIODRUG AG; HEISER, Ulrich; BUCHHOLZ, Mirko; SOMMER, Robert; DEMUTH, Hans-Ulrich; WO2014/140279; (2014); A1;,
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Related Products of 2854-16-2, 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. 2854-16-2, name is 1-Amino-2-methylpropan-2-ol. A new synthetic method of this compound is introduced below.

To a solution of 2-bromobenzaldehyde (25 g, 135 mmol) in methanol (250 mL) was added l-amino-2-methylpropan-2-ol (12.04 g, 135 mmol) and NaOH (13.51 mL, 13.51 mmol). The reaction mixture was stirred under nitrogen atmosphere for 1 h. Then NaBH4 (4.09 g, 108 mmol) was added portion wise for 10 min. It was stirred at 25 °C for 40 h. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (500 mL) and washed with brine solution (300 mL). The organic layer was dried over anhydrous Na2S04, filtered and concentrated to give the title compound (28 g, 108 mmol, 80 percent yield). NMR (DMSO-d6, 400MHz): delta = 7.55 (ddd, J=19.7, 7.7, 1.1Hz, 2H), 7.33-7.39 (m, 1H), 7.18 (td, J=7.6, 1.6 Hz, 1H), 4.19 (s, 1H), 3.78 (s, 2H), 2.40 (s, 2H), 1.99 (s, 1H), 1.03-1.13 ppm (m, 6H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2854-16-2, 1-Amino-2-methylpropan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ASTEX THERAPEUTICS LIMITED; BUDZIK, Brian W; LI, Peng; PERO, Joseph E.; GRIFFITHS-JONES, Charlotte Mary; HEIGHTMAN, Thomas Daniel; NORTON, David; WILLEMS, Hendrika Maria Gerarda; WOOLFORD, Alison Jo-Anne; (176 pag.)WO2018/109642; (2018); A1;,
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Electric Literature of 14320-38-8, Adding some certain compound to certain chemical reactions, such as: 14320-38-8, name is Cyclopent-3-enol,molecular formula is C5H8O, 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 14320-38-8.

Step 1: Toluene-4-sulfonic acid cyclopent-3-enyl ester Cyclopent-3-ene-1-ol (200 mg, 2.38 mmol) was dissolved in pyridine (2.5 ml) and p-toluenesulfonyl chloride (558 mg, 2.92 mmol) was added portionwise at 0 C. After the addition was completed the reaction mixture was stirred at 0 C. for 3 h and then kept in the fridge overnight. Then it was poured into to a mixture of ice and diluted HCl (pH ~5). The solid was filtered off, washed with diluted HCl and dried to obtain the title compound as off-white solid (447 mg, 79%). MS (EI): 256.2 (M+NH4)+.

According to the analysis of related databases, 14320-38-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Banner, David; Ceccarelli, Simona M.; Grether, Uwe; Haap, Wolfgang; Hilpert, Hans; Kuehne, Holger; Mauser, Harald; Plancher, Jean-Marc; Sanchez, Ruben Alvarez; US2010/317647; (2010); A1;,
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Synthetic Route of 109-83-1, 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 109-83-1, name is 2-(Methylamino)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

A solution of 4-methoxy-2,3,6-trimethylbenzenesulfonyl chloride (2.29 g, 9.19 mmol) in THF (30 ml) was added dropwise to a solution of 2-methyl- aminoethanol (0.89 g, 0.95 ml, 11.8 mmol) and Et3N (5 ml) in THF (15 ml) at O 0C. The mixture was subsequently stirred at RT for 5 h and then concentrated in vacuo, the residue was taken up in NaHCO3 solution, and the mixture was extracted with EtOAc (3 x 30 ml). The combined organic phases were dried with Na2SO4 and concentrated in vacuo. Yield: 2.38 g (90 %)

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 109-83-1, 2-(Methylamino)ethanol.

Reference:
Patent; GRUeNENTHAL GMBH; WO2009/109364; (2009); A1;,
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Synthetic Route of 2566-44-1, 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 2566-44-1 as follows.

A solution of diisopropyl (E)-diazene-l,2-dicarboxylate (0.024 mF, 0.121 mmol) in (0305) THF (0.2 mF) was added dropwise to a mixture ofN-((S)-l-((3P)-3-(4-chloro-l-(2,2- difluoroethyl)-3-(N-(4-methoxybenzyl)methylsulfonamido)-lH-indazol-7-yl)-7-hydroxy-4- oxo-3,4-dihydropyrido[2,3-d]pyrimidin-2-yl)-2-(3,5-difluorophenyl)ethyl)-2-((3bS,4aR)-3- (difluoromethyl)-5,5-difluoro-3b,4,4a,5-tetrahydro-lH-cyclopropa[3,4]cyclopenta[l,2- c]pyrazol-l-yl)acetamide (0.04 g, 0.040 mmol), 2-cyclopropylethan-l-ol (10.42 mg, 0.121 mmol) and triphenylphosphine (0.034 g, 0.129 mmol)in Tetrahydrofuran (THF) (0.8 mL) at rt. The reaction mixture was stirred for 18 h at ambient temperature. The reaction mixture was stirred for 18 h and then concentrated in vacuo. The crude residue was taken up in DCM (0.5 mL) and TFA (0.25 mL). Triflic acid (8.48 pL, 0.096 mmol) was added. The resultant purple solution was stirred for 1 h and then concentrated in vacuo. The crude residue was taken up in ethyl acetate (1.5 mL), washed with saturated aqueous NaHCCh (1 mL), and concentrated in vacuo. The crude product was purified by preparatory HPLC using the following conditions: Column: Zorbax Eclipse Plus C18, 21.2 x 100 mm, 5 pm particles; Solvent A = 0.1% Formic Acid in 100% Water. Solvent B = Acetonitrile. Flow Rate = 40 mL/min. Start % B = 59.4 Final % B = 79.4. Gradient Time = 7 min, then a 2 min hold at 98% B. Wavelength = 215 and 254 nm. ESI + Range: 150 to 1500 dalton. Sample was loaded at 59.4% B and afforded N-((S)-l-((3P)-3-(4-chloro-l-(2,2-difluoroethyl)-3- (methylsulfonamido)-lH-indazol-7-yl)-7-(2-cyclopropylethoxy)-4-oxo-3,4- dihydropyrido [2,3 -d]pyrimidin-2-yl)-2-(3 ,5 -difluorophenyl)ethyl)-2-((3bS,4aR)-3 – (difluoromethyl)-5,5-difluoro-3b,4,4a,5-tetrahydro-lH-cyclopropa[3,4]cyclopenta[l,2- c]pyrazol-l-yl)acetamide (0.0041 g, 4.14 pmol, 10 % yield). NMR (500 MHz, (0306) METHAN OL-d4) d ppm 8.42 – 8.53 (m, 1 H) 7.21 – 7.40 (m, 2 H) 7.00 – 7.13 (m, 1 H) 6.55 – 6.83 (m, 4 H) 5.88 – 6.18 (m, 1 H) 5.50 – 5.71 (m, 2 H) 4.53 – 4.79 (m, 5 H) 4.30 – 4.42 (m, 1 H) 3.87 – 4.00 (m, 1 H) 3.39 – 3.45 (m, 1 H) 3.23 – 3.26 (m, 3 H) 3.06 – 3.13 (m, 1 H) 2.55 – 2.62 (m, 1 H) 2.40 – 2.47 (m, 2 H) 1.70 – 1.74 (m, 3 H) 1.35 – 1.39 (m, 2 H) 0.99 – 1.04 (m, 1 H). LC/MS retention time = 1.40 min; m/z = 932.2 [M+H]+ Column: Acquity BEH C 18, 2.1 x 30 mm, 1.7 pm particles; Solvent A = 0.1% Formic acid in 100% Water. Solvent B = 0.1% Formic Acid in 100% Acetonitrile. Flow Rate = 0.8 mL/min. Start % B = 5. Final % B = (0307) 95. Gradient Time = 1.7 min, then a 0.2 min hold at 95% B. Wavelength = 215 and 254 nm. ESI+ Range: 150 to 1500 Dalton. System: Agilent 1290 Infinity II

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2566-44-1, its application will become more common.

Reference:
Patent; VIIV HEALTHCARE UK (NO.5) LIMITED; IWUAGWU, Christiana; PEESE, Kevin M.; (0 pag.)WO2020/58844; (2020); A1;,
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