Month: July 2021

Adding a certain compound to certain chemical reactions, such as: 4845-50-5, 1,4-Dioxane-2,3-diol, 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: 1,4-Dioxane-2,3-diol, blongs to alcohols-buliding-blocks compound. Recommanded Product: 1,4-Dioxane-2,3-diol

4.00 g (19.509 mmol) of the compound from example 89A was dissolved in 100 ml ethanol and 2.42 g (19.509 mmol) of 2,3-dihydroxy-l,4-dioxane was added. The mixture was stirred for 4 h at room temperature and a further 2.42 g (19.509 mmol) of 2,3-dihydroxy-l,4-dioxane was added. After stirring for 24 h at room temperature, the mixture was concentrated in a rotary evaporator and the residue was purified by silica-gel chromatography (eluent: dichloromethane/methanol = 30:1). We obtained 3.60 g (80% of theor.) of the target compound.LC-MS (method 1): R, = 1.79 min; MS (EIpos): m/z = 227 [M+H]+.1H-NMR (400 MHz, DMSO-D5): delta [ppm] = 8.06 (dd, IH), 8.24 (t, IH), 9.05 (d, IH), 9.07 (d, IH).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,4845-50-5, 1,4-Dioxane-2,3-diol, and friends who are interested can also refer to it.

Reference:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; BAeRFACKER, Lars; KAST, Raimund; GRIEBENOW, Nils; MEIER, Heinrich; KOLKHOF, Peter; ALBRECHT-KUePPER, Barbara; NITSCHE, Adam; STASCH, Johannes-Peter; SCHNEIDER, Dirk; TEUSCH, Nicole; RUDOLPH, Joachim; WHELAN, James; BULLOCK, William; PLEASIC-WILLIAMS, Susan; WO2010/20363; (2010); A1;,
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Synthetic Route of 15852-73-0, 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.15852-73-0, name is (3-Bromophenyl)methanol, molecular formula is C7H7BrO, molecular weight is 187.03, as common compound, the synthetic route is as follows.

Example 53 {[(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), then 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, the mixture was warmed to room temperature, and stirred for 2 h. 5% HCl was added to the reaction mixture to pH=4-5, then the organic phase was separated, and the aqueous layer was extracted with CH2Cl2 (50 mL*2). The combined organic phase was 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%).

Statistics shows that 15852-73-0 is playing an increasingly important role. we look forward to future research findings about (3-Bromophenyl)methanol.

Reference:
Patent; Glaxo Group Limited; US2009/197871; (2009); A1;,
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Application of 68120-35-4, Adding some certain compound to certain chemical reactions, such as: 68120-35-4, name is (3-Bromo-4-methylphenyl)methanol,molecular formula is C8H9BrO, 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 68120-35-4.

A mixture of (3-Bromo-4-methyl-phenyl)-methanol (8.5 g, 42.2 mmol) and bis(pinacolato)diboron (11.8 g, 46.50 mmol) in 1 ,4-dioxane (50 ml_) was degassed under N2 atmosphere for 10 min. Potassium acetate (8.2 g, 84.55 mmol) was added to the above followed by [1 ,1 – Bis(diphenylphosphino)ferrocene]dichloropalladium(ll).CH2Cl2 (1.54 g, 2.11 mmol) and the reaction mixture was heated at 100 C for 15 h. The solvents were removed under reduced pressure, the residue obtained was diluted with water and extracted with EtOAc (2×150 mL). Combined organic phases were washed with water, brine, dried over anhydrous Na2S04, filtered and concentrated. Purification of this crude by flash chromatography on silica (EtOAc:n-hexane; 70:30) afforded the title compound as a brown liquid (5.0 g, 84%). 1H NMR (400 MHz, DMSO-d6): delta 7.59 (d, J = 1.72 Hz, 1 H), 7.25 (dd, J = 7.76, 1.88 Hz, 1 H), 7.11 (d, J = 7.76 Hz, 1 H), 5.10 (t, J = 5.72 Hz, 1 H), 4.43 (d, J = 5.72 Hz, 2H), 2.42 (s, 3H), 1.29 (s, 12H).

According to the analysis of related databases, 68120-35-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK PATENT GMBH; JORAND-LEBRUN, Catherine; KULKARNI, Santosh; CHRISTMANN-FRANCK, Serge; WO2014/121942; (2014); A1;,
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Synthetic Route of 86770-74-3 ,Some common heterocyclic compound, 86770-74-3, molecular formula is C8H19NO4, 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 2-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)ethanol (256 mg, 1.32 mmol) in DCM (30 mL) were added BCN-OSu (351 mg, 1.20 mmol) and Et3N (502 muIota_, 364 mg, 3.60 mmol). The resulting solution was stirred for 30 min and washed with a saturated aqueous solution of NH4CI. After separation, the aqueous phase was extracted with DCM (30 mL). The combined organic phases were dried (Na2S04) and concentrated. The residue was purified with column chromatography (MeOH in DCM 0? 10%). The product was obtained as a colourless oil (397 mg, 1.07 mmol, 90%). H NMR (400 MHz, CDCI3) delta (ppm) 5.93 (bs, 1 H), 4.14 (d, J = 8.1 Hz, 2H), 3.77-3.69 (m, 4H), 3.68-3.59 (m, 8H), 3.58-3.52 (m, 2H), 3.42-3.32 (m, 2H), 2.34-2.16 (m, 6H), 1.66-1.51 (m, 2H), 1 .36 (quintet, J = 8.7 Hz, 1 H), 1.00-0.85 (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. 86770-74-3, 2-(2-(2-(2-Aminoethoxy)ethoxy)ethoxy)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SYNAFFIX B.V.; VERKADE, Jorge Merijn Mathieu; WIJDEVEN, Maria Antonia; VAN DE SANDE, Petrus Josephus Jacobus Maria; VAN GEEL, Remon; VAN DELFT, Floris Louis; VAN BERKEL, Sander Sebastiaan; (117 pag.)WO2017/137456; (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. 71176-54-0, name is (5-Amino-1,3-phenylene)dimethanol, the common compound, a new synthetic route is introduced below. Quality Control of (5-Amino-1,3-phenylene)dimethanol

Compound 3d (5.6 g, 18.52 mmol) was dissolved in anhydrous dichloromethane (1 18 mL) and anhydrous methanol (58.8 mL). (5-amino-1 ,3- phenylene)dimethanol (2.70 g, 17.64 mmol) and EEDQ (8.72 g, 35.3 mmol) were then added, and the reaction was stirred at room temperature overnight. The solvent was stripped and ethyl acetate was added. The resulting slurry was filtered, washed with ethyl acetate, and dried under vacuum/N2 to give compound 3e (2.79 g, 36% yield). 1 H NMR (400 MHz, DMSO-d6): delta 9.82 (s, 1 H), 8.05, (d, 1 H, J = 9.2 Hz), 8.01 (d, 1 H, J = 7.2 Hz), 7.46 (s, 2H), 6.95 (3, 1 H), 5.21 -5.12 (m, 2H), 4.47-4.42 (m, 4H), 4.40-4.33 (m, 1 H), 4.33-4.24 (m, 1 H), 3.58 (s, 3H), 2.33-2.26 (m, 2H), 2.16-2.09 (m, 2H), 1 .54-1 .46 (m, 4H), 1 .30 (d, 3H, J = 7.2 Hz), 1 .22 (d, 3H, J = 4.4 Hz).

The synthetic route of 71176-54-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MILLENNIUM PHARMACEUTICALS, INC.; IMMUNOGEN, INC.; VEIBY, Ole Peter; CHARI, Ravi, V. J.; LAMBERT, John M.; LAI, Katharine C.; HERBST, Robert W.; HILDERBRAND, Scott A.; (128 pag.)WO2017/136693; (2017); A1;,
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Adding a certain compound to certain chemical reactions, such as: 111-45-5, 2-(Allyloxy)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, Product Details of 111-45-5, blongs to alcohols-buliding-blocks compound. Product Details of 111-45-5

Reactions under ambient pressure: In a glove box, a 4 ml_ vial equipped with a magnetic stirring bar and a screw cap was charged with the substrate (0.1 mmol) and 2 mg of hexamethylbenzene (internal standard). Then a solution of the catalyst (5×10″3 mmol, 5 mol %) dissolved in the right amount of toluene to achieve the final concentration of 1 M in substrate, was added to the vial containing the substrate and the internal standard. The vial was closed and the reaction mixture was stirred at room temperature (22 SC). Samples (about 10 mu_) of the reaction mixture were withdrawn at regular time intervals, and quenched with an excess of ethyl vinyl ether. Determination of conversions, yields, and Z-selectivities were carried out by comparing the integrals of the peaks due to the olefinic protons of substrates and products, identified by comparison with literature data,( 20, 37-41 ) with that of the internal standard.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,111-45-5, 2-(Allyloxy)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; BERGEN TEKNOLOGIOVERFØRING AS; JENSEN, Vidar Remi; OCCHIPINTI, Giovanni; (64 pag.)WO2017/9232; (2017); A1;,
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Reference of 7218-43-1 ,Some common heterocyclic compound, 7218-43-1, molecular formula is C7H12O3, 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.

120mg NaH (60%) was added to a solution of 144mg 1-propargyl diethylene glycol in 5mL THF,Stir at room temperature for 15 minutes, then add 152 mg of bromoacetic acid and heat to reflux for 6 hours.After the reaction was completed, 10 mL of saturated ammonium chloride solution was added to quench the reaction, and the organic phase was separated.The aqueous phase was extracted three times with dichloromethane and incorporated into the organic phase,It was washed successively with saturated aqueous ammonium chloride solution and saturated brine, and then dried over anhydrous sodium sulfate,The sodium sulfate was removed by filtration and concentrated to obtain the crude product.The crude product was isolated by column chromatography (200-300 mesh silica gel, eluent dichloromethane: methanol = 50: 1) to obtain pure intermediate 26.

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. 7218-43-1, 2-[2-(2-Propynyloxy)ethoxy]ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ShanghaiTech University; Tao Houchao; Zhao Fei; (85 pag.)CN110894209; (2020); A;,
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Application of 5187-23-5, Adding some certain compound to certain chemical reactions, such as: 5187-23-5, name is (5-Ethyl-1,3-dioxan-5-yl)methanol,molecular formula is C7H14O3, 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 5187-23-5.

Example 12: Synthesis of Tetradecafluoro-di(propylamino)- phthalocyaninatocobalt(II), Dodecafluoro-tetrapyrrolidino-phthalocyaninatocobalt(II) and MONO- (5-ETHYL-1, 3-DIOXANE-5-METHYLOXY)-HEXAFLUORO-TETRANEOPENTOXY-PENTAPYRROLIDIYAO- phthalocyaninatocobalt (II) [00129] FI6COPC (40 mg) was dissolved in 1 ml of propylamine and stirred for 10 min. Then the amine was evaporated and an aliquot was taken for MALDI-MS. It shows substitution of 1-6 fluorines by propylamine. To the remaining solid 1 ml of pyrrolidine was added and the suspension was stirred at room temperature for 5 min. After that the pyrrolidine was evaporated and an aliquot was taken for MALDI-MS. It shows substitution of 3-4 fluorines by pyrrolidine but no more products with propylamine as the substituent. To the remaining solid 1 ml of diisopropylamine was added and the mixture was heated to 80C for 4 hrs. The amine was evaporated and an aliquot taken for MALDI-MS. It shows substitution of 3-5 fluorines by pyrrolidine. There is no evidence that diisopropylamine has reacted with the Pc. To the remaining solid (dark blue green) was added a mixture of 0.93 ml nBuLi and 328 mg neopentylalcohol. The mixture was stirred at 110C for 90 min. Since the suspension almost solidified, some 5-ethyl-1, 3-dioxane-5-methanol was added and heated to 140C for 1 h. The colour turned from green to brown. But after cooling down it was green again. So another 328 mg neopentylalcohol were added and heated to 140C for 90 min. The colour turned brown again. The mixture was purified by silica gel chromatography with ethylacetate/hexanes (1: 1) as the eluent. An olive green and a green fraction were taken and submitted for MALDI-MS. Two peaks among several could be identified: [00130] 1) fluorines were replaced by 5 pyrrolidines and 4 neopentylalcohols [00131] 2) the same as above with an 5-ethyl-1, 3-dioxane-5-methanoxy. [00132] The reaction schemes for the synthesis of the various products of this example are provided in Figure 7.

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. 5187-23-5, (5-Ethyl-1,3-dioxan-5-yl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; YORK UNIVERSITY; WO2005/33110; (2005); A1;,
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Application of 23377-40-4, Adding some certain compound to certain chemical reactions, such as: 23377-40-4, name is 3-(Hexadecyloxy)propan-1-ol,molecular formula is C19H40O2, 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 23377-40-4.

General procedure: 4.1. General method A Bis isopropyl phosphonoethoxyethylchloride (1) (2.58 g,10.0 mmol) or bis isopropyl phosphonomethyltosylate (7) (3.50 g,10.0 mmol) in anhydrous acetonitrile (130 ml) was treated withbromotrimethylsilane (13 ml) overnight at room temperature.The mixture was then evaporated and codistilled with acetonitrile (3×25 mL), water (2×25 ml), ethanol (25 mL) and toluene (3 x 25 mL). The syrupy residue was dissolved in dichloromethane (50 ml) then DMF (0.1 ml) and oxalyl chloride (6.0 ml, 68.8 mmol) were added. The solution was gently refluxed (2 h), evaporated to dryness, and redissolved in dichloromethane (20 ml). The solution was cooled down to 0 C and treated slowly with pyridine (1.6 ml).The mixture was added to a cooled ( 30 C) solution of hexadecyloxypropanol (6.01 g, 20 mmol) in dichloromethane (100 ml) and triethylamine (8.7 ml). The mixture was allowed to reach 0C and kept at this temperature for3 h.The reactionmixturewas evaporated,codistilled with toluene (3 50 ml) and the residue was chromatographed on a silica gel column (400 g) in EtOAc/hexane (1:2/1:1). 4.1.1. Bis(hexadecyloxypropyl)phosphonoethoxyethylchloride (2) Yield 6.50 g of syrup (88%). The crude product was used without further purification procedures. ESI-MS, m/z: 753.6 (53) [M th H]th, 775.6 (100) [M th Na]th, 791.5 (22) [M th K]th, 812.7 (28); ESI-HRMS calcd for C42H87O6ClP 753.59233, found: 753.59185 [M th H]th.

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. 23377-40-4, 3-(Hexadecyloxy)propan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Tichy, Tomas; Dracinsky, Martin; Krecmerova, Marcela; Andrei, Graciela; Snoeck, Robert; Balzarini, Jan; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 307 – 314,8;; ; Article; Tichy, Tomas; Andrei, Graciela; Snoeck, Robert; Balzarini, Jan; Dracinsky, Martin; Krecmerova, Marcela; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 307 – 314;,
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Synthetic Route of 647-42-7, 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 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

C6F13-CH2CH2-O-CH2CH=CH2197.11g (488mmol) was dropped in 2 hours. It agitated at 110 degrees C after the end of dropping for 2 hours. Then, it lowered to 70 degrees C. NaOH solution 25.07g was added 0.1%, and it stirred for 2 hours. drying in 60 degrees C / 5KPa — after the end of drying, and the temperature — cull — bora — fin 3(made in Japanese Emba Illo Kem Carzou)2.51g was added, and it stirred for 2 hours. It filtered with the 0.1micrometer PTFE membrane filter, steam distillation of the filtrate was carried out using 100 degrees C / 5KPa, and the water 62.5g, and 206.3 g of object compounds (compound B1) were obtained (89% of yield).

According to the analysis of related databases, 647-42-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; KAO CORPORATION; WATARAI, ETSUKO; IGARASHI, TAKANORI; YAGO, YUKO; UEHARA, KOICHI; (20 pag.)JP2017/25048; (2017); A;,
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