Tag: M.W=100-200

870-72-4, Adding a certain compound to certain chemical reactions, such as: 870-72-4, Hydroxymethanesulfonic Acid Sodium Salt, 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, 870-72-4, blongs to alcohols-buliding-blocks compound.

EXAMPLE 4 [0188] 422 parts of 4-(beta-sulfatoethylsulfonyl)aniline are suspended in 1000 parts of ice-water and 270 parts of 30% hydrochloric acid and diazotized by dropwise addition of 260 parts of 40% sodium nitrite solution. After excess nitrite has been removed with sulfamic acid solution, the diazo suspension obtained is admixed with an aqueous solution of 166.5 parts of 4-hydroxy-7-(sulfomethylamino)naphthalene-2-sulfonic acid (obtained by reaction of 119.5 parts of 7-amino-4-hydroxynaphthalene-2-sulfonic acid with 75 parts of formaldehyde sodium bisulfite in an aqueous medium at pH 5.5-6 and 45 C.) and adjusted to pH 1.5 with solid sodium bicarbonate. After the acidic coupling has ended, this reaction mixture has added to it an aqueous solution of 335 parts of the second coupling component (18-1) and is adjusted to and maintained at pH 5-6 with sodium carbonate below 25 C. [C00035] [00035] [0189] The 50:50 mixture of the two dyes (1-4) and (11-3) which has formed after the coupling reaction has ended can be isolated by evaporation under reduced pressure or by spray drying. [C00036] [00036] [0190] The resulting dye mixture according to the present invention dyes cotton in red shades.; EXAMPLE 11 [0206] 281 parts of 4-(beta-sulfatoethylsulfonyl)aniline are suspended in 700 parts of ice-water and 180 parts of 30% hydrochloric acid and diazotized by dropwise addition of 173 parts of 40% sodium nitrite solution. After excess nitrite has been removed with sulfamic acid solution, the diazo suspension obtained is admixed with an aqueous solution of 83 parts of 4-hydroxy-7-(sulfomethylamino)naphthalene-2-sulfonic acid (obtained by reaction of 60 parts of 7-amino-4-hydroxynaphthalene-2-sulfonic acid with 37.5 parts of formaldehyde sodium bisulfite in an aqueous medium at pH 5.5-6 and 45 C.) and adjusted to pH 1.5 with solid sodium bicarbonate. After the acidic coupling has ended, this reaction mixture has added to it an aqueous solution of 111 parts of 4-amino-phthalene-1-sulfonic acid as the second coupling component and is adjusted to and maintained at pH 5-6 with sodium carbonate below 25 C. After the coupling reaction has ended, the reaction mixture is admixed with 73 parts of the golden yellow azo dye of the formula (Ga-1) and the resulting 42:46:12 mixture of the three azo dyes (I-4), (II-6) and (Ga-1) is isolated by spray drying. [C00046] [00046] [0207] The resulting dye mixture according to the present invention provides orange dyeings and prints on cotton for example under the dyeing conditions customary for reactive dyes.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,870-72-4, its application will become more common.

Reference:
Patent; DyStar Textilfarben GmbH & Co. Deutschland KG; US2005/34253; (2005); A1;,
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3360-41-6, 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 3360-41-6, name is 4-Phenylbutan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

To a mixture of 5 ml (32.75 mmol) 4-phenylbutanol with 10.1 ml (65.66 mmol) 1,6-dibromohexane is added 8 g (121.2 mmol) powdered KOH and 1.112 g (3.28 mmol) tetrabutylammonium hydrogen sulfate. After allowing the suspension to stir for 20 hr at room temperature, it is filtered and the filtrate dissolved in 50 ml Et2O. The resulting solution is washed with water, dried on anhydrous Na2SO4, the Et2O evaporated and the residue distilled in vacuum (0.1 mmHg), a first fraction up to 100 C. of a mixture of starting products and a second fraction at 150 C. of 4-(6-bromohexyloxy)butylbenzene weighing 7.60 g (74.4 %) being collected. RMN 1H (CDCl3), delta (ppm): 1.3-2.0 (m, 12H), 2.6 (t, 2H, -CH2-C6H5), 3.4 (m, 6H, -CH2-O-CH2-+-CH2Br), 7.1-7.4 (m, 5H, -C6H5).

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 3360-41-6, 4-Phenylbutan-1-ol.

Reference:
Patent; Bessa Bellmunt, Jordi; Dalmases Barjoan, Pere; Marquillas Olondriz, Francisco; US6388134; (2002); B1;,
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873-63-2, 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.873-63-2, name is 3-Chlorobenzyl alcohol, molecular formula is C7H7ClO, molecular weight is 142.58, as common compound, the synthetic route is as follows.

General procedure: A 50 mL round bottom flask was charged with a mixture of aryl chloride (0.5 mmol), arylboronic acid (0.75 mmol), K2CO3 (1.5 mmol), Pd catalyst (0.2 mol %), solvent (6 mL) and the mixture was stirred for required times at appropriate temperature. After completion, the reaction mixture was diluted with water (20 mL) and extracted with ether (20 mL ¡Á3). Combined extract was washed with brine (20 mL ¡Á3) and dried over Na2SO4. After evaporation of the solvent under reduced pressure, the residue was chromatographed (silica gel, ethyl acetate/hexane 1:9) to obtain the desired product. The products were confirmed by comparing the melting points, 1H NMR and mass spectral data with authentic samples.

Statistics shows that 873-63-2 is playing an increasingly important role. we look forward to future research findings about 3-Chlorobenzyl alcohol.

Reference:
Article; Shahnaz, Nasifa; Banik, Biplab; Das, Pankaj; Tetrahedron Letters; vol. 54; 22; (2013); p. 2886 – 2889;,
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Adding a certain compound to certain chemical reactions, such as: 770-71-8, Adamantan-1-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, 770-71-8, blongs to alcohols-buliding-blocks compound. 770-71-8

Example 57A 1-(azidomethyl)tricyclo[3.3.1.13,7]decane 1-Adamantanemethanol (500 mg) was dissolved in dichloromethane (15 mL). The solution was chilled in an ice bath and triethylamine (0.587 mL) was added, followed by methanesulfonyl chloride (0.258 mL). The reaction mixture was stirred for 4 hours at 0 C., then transferred to a separatory funnel and rinsed with 1N aqueous HCl (15 mL), saturated aqueous NaHCO3 (15 mL) and brine (15 mL). The organic extracts were dried (Na2SO4), filtered, and concentrated. A portion of the resulting crude mesylate (293 mg) and sodium azide (390 mg) were combined in N,N-dimethylformamide (1.2 mL) and the reaction mixture was heated to 120 C. overnight, then cooled to room temperature and partitioned between ethyl acetate (3*15 mL) and water (20 mL). The organic extracts were dried (Na2SO4), filtered, and concentrated to provide the title compound, which was used in the next step without further purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,770-71-8, its application will become more common.

Reference:
Patent; AbbVie Inc.; WANG, LE; Doherty, George; Wang, Xilu; Tao, Zhi-Fu; Bruncko, Milan; Kunzer, Aaron R.; Wendt, Michael D.; Song, Xiaohong; Frey, Robin; Hansen, Todd M.; Sullivan, Gerard M.; Judd, Andrew; Souers, Andrew; US2013/96120; (2013); A1;,
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101-98-4, A common compound: 101-98-4, name is 2-(Benzyl(methyl)amino)ethanol,molecular formula is C10H15NO, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

A 500 mL flask (reactor flask) was charged with N-benzyl-N-methylethanolamine (24.5 mL), DCM (120 mL), NaOH (80 mL; 30 wt %) and tetrabutylammonium chloride. Mixing at low speed throughout the reaction, the mixture was cooled to -10 C. (cooling bath), and the addition funnel charged with DCM (30 mL) and mesyl chloride (15.85 mL), which was added drop wise at a constant rate over 30 minutes. The addition was exothermic, and stirring was continued for 15 minutes while the temperature equilibrated back to -10 C. The reaction was held for at least 10 minutes to ensure full hydrolysis of the excess mesyl chloride.A 250 mL flask was charged with biphenyl-2-ylcarbamic acid piperidin-4-yl ester (26 g; prepared as described in Preparation 3) and DCM (125 mL), stirred for 15 minutes at room temperature, and the mixture chilled briefly to 10 C. to form a slurry. The slurry was then charged into the reactor flask via the addition funnel. The cooling bath was removed and the reaction mixture was warmed to 5 C. The mixture was transferred to a separatory funnel, the layers allowed to settle, and the aqueous layer removed. The organic layer was transferred back to the reactor flask, stirring resumed, the mixture held to room temperature, and the reaction monitored by HPLC for a total of 3.5 hours.The reactor flask was charged with NaOH (1M solution; 100 mL), stirred, and the layers allowed to settle. The organic layer was separated, washed (NaCl saturated solution), its volume partially reduced under vacuum, and subjected to repeated IPA washings. The solids were collected and allowed to air-dry (25.85 g, 98% purity). Additional solids were obtained from further processing of the mother liquor (volume reduction, IPA, cooling).

With the rapid development of chemical substances, we look forward to future research findings about 101-98-4.

Reference:
Patent; Mu, YongQi; Dalziel, Sean M.; Ji, Yu-Hua; Preza, Leticia Maria; US2008/58374; (2008); A1;,
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770-71-8, 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.770-71-8, name is Adamantan-1-ylmethanol, molecular formula is C11H18O, molecular weight is 166.26, as common compound, the synthetic route is as follows.

General procedure: To a solution of alcohol (1 mmol) in MeCN-H2O (9:1, 3 mL) were successively added TEMPO (7.8 mg,5 mol%), NH4OAc (0.308 g, 4 equiv), and PhI(OAc)2 (0.708g, 2.2 equiv). The suspension was stirred at roomtemperature (progress of the reaction was monitored byTLC) for the reaction time indicated in Table 2. The resultantclear two-phase reaction mixture was concentrated, dilutedwith H2O and Et2O, and the organic layer was dried (Na2SO4), filtered, and evaporated under reduced pressure.The residue was purified by flash column chromatography(PE-Et2O or PE-CH2Cl2) to give 2.

Statistics shows that 770-71-8 is playing an increasingly important role. we look forward to future research findings about Adamantan-1-ylmethanol.

Reference:
Article; Vatele, Jean-Michel; Synlett; vol. 25; 9; (2014); p. 1275 – 1278;,
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100-37-8, 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. 100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, 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.

Example 32; N-cyclopropyl-3-({4-[(6-{ [2-(diethylamino) ethoxy] methyl} pyridin-2- yl) methoxy] benzoyl} amino)-4-methylbenzamide To a 60% dispersion of NaH in mineral oil (25 mg, 0.625 mmol) in DMA (4 mL) was added N,N-diethylethanolamine (24 mg, 0.205 mmol). The reaction was stirred at room temperature for 20 minutes. A solution of 3- [ (4- { [6- (bromomethyl) pyridin-2- yl] methoxy benzoyl) amino]-N-cyclopropyl-4-methylbenzamide (77 mg, 0.155 mmol) in DMA (2 mL) was added dropwise to the reaction which was then stirred for 1 h at room temperature. The reaction was quenched by the addition of water (1 mL) and was purified by preparative HPLC to give the title compound as a white solid (29 mg, 35%); NMR Spectrum: (DMSOd6) 0.58 (m, 2H), 0.69 (m, 2H), 0.96 (t, 6H), 2.26 (s, 3H), 2.50 (m, 4H), 2.64 (t, 2H), 2.86 (m, 1H), 3.59 (t, 2H), 4.59 (s, 2H), 5.75 (s, 2H), 7.18 (d, 2H), 7.33 (d, 1H), 7.42 (m, 2H), 7.64 (dd, 1H), 7.80 (s, 1H), 7. 87 (t, 1H), 7.96 (d, 2H), 8. 36 (d, 1H), 9.83 (s, 1H) ; Mass Spectrum : M+H+ 531.

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. 100-37-8, 2-(Diethylamino)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2005/61465; (2005); A1;,
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623-72-3, 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. 623-72-3, name is Ethyl 3-Hydroxypropanoate. This compound has unique chemical properties. The synthetic route is as follows.

Example 16 This example describes the preparation of various alkyl acrylate esters by dehydrating 3-HP esters using various catalysts. A catalyst was placed in a 3-neck flask that was equipped with a temperature probe (in contact with the catalyst). A distillation column and receiving flask were attached so that the vapors formed during the reaction could be collected, and the catalyst was heated to the desired temperature. A solution of a 3-hydroxypropionic acid ester in the corresponding alcohol was added drop-wise directly onto the catalyst using a syringe. The liquid that distilled over was collected and analyzed by gas chromatography. The results, and corresponding experimental conditions are shown in the following table. Ester Catalyst Temperature Concentration Solvent Yield of Yield of (C) of Ester in Acrylic Acrylic Solvent ester (GC) acid (GC) – (%) (%) (%) Ethyl NaH2P04-Silica 275-EtOH 49 26 Ethyl NaH2PO4-Silica 250 35 EtOH 53 Ethyl NaH2PO4-Silica 250 50 EtOH 14 21 Ethyl NaH2PO4-Silica 180 40 EtOH 30 – Ethyl Copper-H3PO4 220 20 EtOH 50 50 Methyl NaH2PO4-Silica 280-MeOH 78 Methyl CuS04-Silica 280-MeOH 37 9 Methyl Cs2CO3-Silica 220 45 MeOH 49 – Butyl NaH2PO4-Silica 280 50 BuOH 40 Similar dehydration reactions were performed using 3-HP as the starting material and a flask containing heated catalyst in place of the GC: (a) Aqueous 3-HP was dehydrated to acrylic acid over NaH2PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 90- 96%. (b) Aqueous 3-HP was dehydrated to acrylic acid over H3PO4-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 85-90%. (c) Aqueous 3-HP was dehydrated to acrylic acid over CuS04-Silica gel catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 73%. (d) Aqueous 3-HP was dehydrated to acrylic acid over Zeolite H-ss powder and 85% H3PO4 as the catalyst at 180C. Based on GC and HPLC analysis, the yield of acrylic acid was 71%. (e) Aqueous 3-hydroxyisobutyric acid was dehydrated to methacrylic acid over NaH2PO4-Silica gel catalyst at 270C. Based on GC analysis, the yield of methacrylic acid was 79%.

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 623-72-3, Ethyl 3-Hydroxypropanoate.

Reference:
Patent; CARGILL, INCORPORATED; WO2003/82795; (2003); A2;,
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Adding a certain compound to certain chemical reactions, such as: 626-18-6, 1,3-Benzenedimethanol, 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, 626-18-6, blongs to alcohols-buliding-blocks compound. 626-18-6

To a stirred solution of 1, 3-phenylenedimethanol (1) (5 g, 36.496 mmol) in THF (100 mL) was treated with NaH (1.17 g, 29.197 mmol) at 0C to RT for 30 min. Ethyl iodide (2.3 ml, 29.197 mmol) in THF (10 mL) was added to above reaction mixture at OC and stirred at 50 C for 16h under nitrogen atmosphere. The reaction mixture was quenched with ice water and extracted with ethyl acetate (3x100mL). Combined organic layers were washed with brine (2×100 mL) and dried over Na2SO4, evaporated under reduced pressure. Crude residue was purified by Combi-flash chromatography using 20 % ethyl acetate in pet-ether to afford (3-(ethoxy methyl) phenyl) methanol 3 (2.1g, 12.65 mmol, 34 % yield) as a yellowish oily liquid. TLC system: 40 % ethyl acetate in pet-ether – Rf: 0.50; LCMS: m/z = 120.99 (M-46) +

With the rapid development of chemical substances, we look forward to future research findings about 626-18-6.

Reference:
Patent; COCRYSTAL PHARMA, INC.; JACOBSON, Irina, C.; FEESE, Michael, David; LEE, Sam, Sk; (249 pag.)WO2018/200425; (2018); A1;,
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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 107-75-5, name is 7-Hydroxy-3,7-dimethyloctanal. This compound has unique chemical properties. The synthetic route is as follows. 107-75-5

General procedure: Aldehyde (2 equiv) was added to a mixture of N-acyl phthalimide (1 equiv), potassium phthalimide (20 mg, 0.11 mmol, 0.2 equiv), NaI (16 mg, 0.11 mmol, 0.2 equiv), 4 A MS (100 mg), MeCN (0.53 mL), and EtOAc (0.53 mL) at room temperature with stirring. After 24 h, the mixture was diluted in Et2O, and sequentially washed with satd aq NH4Cl (1¡Á), 1 M aq NaOH (3¡Á), and brine (1¡Á). The organic phase was dried (MgSO4) and concentrated. The crude material was purified by normal phase flash chromatography using a mixture of hexanes/EtOAc eluent.

Statistics shows that 107-75-5 is playing an increasingly important role. we look forward to future research findings about 7-Hydroxy-3,7-dimethyloctanal.

Reference:
Article; Enright, Robert N.; Grinde, Jeffrey L.; Wurtz, Lincoln I.; Paeth, Matthew S.; Wittman, Tekoa R.; Cliff, Emily R.; Sankari, Yessra T.; Henningsen, Lucas T.; Tan, Chuchen; Scanlon, Joseph D.; Willoughby, Patrick H.; Tetrahedron; vol. 72; 41; (2016); p. 6397 – 6408;,
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