Month: June 2021

Adding a certain compound to certain chemical reactions, such as: 112-70-9, 1-Tridecanol, 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: 112-70-9, blongs to alcohols-buliding-blocks compound. Recommanded Product: 112-70-9

EXAMPLE 3 [00079] The following Example describes the condensation esterification of DDDA using methanesulfonic acid catalyst and the preparation of DDDA diester using a mixture of 50 mole % Telomer alcohol-L and 50 mole % Exxal 13. [00080] A 500 mL round bottom flask was charged with 69.06 g DDDA (MW 230.3, 0.3 mole), 130.41 g Telomer alcohol-L (average molecular weight?414, 0.315 mole), 62.37 g Exxal 13 tridecyl alcohol from Exxon (FW?198, 0.315 mole), 0.29 g methanesulfonic acid (MW 96.1, 0.003 mole), and 100 g mixed xylenes. The reaction flask was fitted with an 8 Vigreux column topped with a Dean-Stark trap and condenser. The reaction was heated to reflux to drive off water, which was separated in the Dean-Stark trap, xylene overflow being returned to the reaction flask. The reaction was followed by water removal and by periodic sampling and titration for acid number. [00081] After 10 and ½ hours reaction time, the acid number had decreased to 1.6 mg KOH/g, and the reaction was considered to be complete. [00082] The reaction product was brown. The reaction product was washed, at 70-80 C., with 330 g of 0.2% aqueous sodium hydroxide. Phases were inverted, with a brown aqueous phase on top and the denser ester phase on the bottom. The lower ester phase was very cloudy. After separating the caustic wash, the ester phase was washed three times with 300 mL portions of warm water. The acid number was 0.56 mg KOH/g. [00083] The crude ester was sparged with nitrogen and heated from room temperature to a temperature of 210-220 C. over a period of 90 minutes to remove xylene, water, and other low boilers. [00084] The yield was 215.72 g of a waxy tan solid having an acid number 0.75 mg KOH/g. [00085] The same basic procedure as above was used to prepare other partially fluorinated esters, listed in Table 5. In all cases, the non-fluorinated alcohol was Exxal 13, tridecyl alcohol from Exxon. Due to difficulty obtaining reliable F elemental analysis, ester end groups were also analyzed by 1H NMR. The chemical shift region between 3.5 and 4.5 ppm downfield of tetramethylsilane reveals the CH2 protons attached to the ester oxygen. In the case of Rf, these CH2 protons are cleanly separated and downfield from the CH2 protons of Rh. The relative molar amounts of Rf and Rh can be calculated from the integrals of these two groups. Where elemental analysis and NMR disagree, the NMR method is believed to be more reliable. Table 5. Partially fluorinated esters prepared by condensation esterification using methanesulfonic acid catalyst[TABLE-US-00006] Mole fractionAcid PartiallypartiallynumberWt % FWt %Prepara- Fluorinatedfluorinated(mg(elementalF (bytionDiacidalcoholalcoholKOH/g)analysis)NMR) 9AdipicTelomer0.0250.341.922.6 alcohol-L10AdipicTelomer0.0250.292.253.2 alcohol11AzelaicTelomer0.02501.831.66 Alcohol-L12C14Telomer0.0250.271.391.28 diacidalcohol-L13CorfreeTelomer0.02501.231.39 M1alcohol-L14CorfreeTelomer0.0250.61.321.49 M1alcohol-L15DDDAPoly HEPO0.0250.14.17 alcohol16DDDATelomer0.025 alcohol17DDDATelomer0.0250.552.12.4 alcohol18DDDATelomer0.0250.131.862 alcohol19DDDATelomer0.0230.100 alcohol20DDDATelomer0.024000 alcohol21DDDATelomer0.0250.181.872.1 alcohol-L22DDDATelomer0.1250.243.019.47 alcohol-L23DDDATelomer0.050.2 4.06 alcohol-L24DDDATelomer0.0250.181.821.92 alcohol-L25DDDATelomer0.250.316.6817.3 alcohol-L26DDDATelomer0.50.75134.634.3 alcohol-L27DDDATelomer0.0250.272.363.4 ethoxylate alcohol28SebacicTelomer0.0250.21.581.63 alcohol-L29SubericTelomer0.0250.260.721.91 alcohol-L [00086] FIG. 4 shows the wear and friction performance of a low-F-content material (?2% F), sample 18 in Table 5, in 150N oil. This low-F-content material was completely soluble even at 20% by weight concentration (0.4 wt. percent F). FIG. 5 compares the anti-wear performance of this low-F material to a similar non-fluorinated diester, ditridecyl dodecanedioate (Hatcol 2907, from Hatco), showing the significant improvement in wear performance from only a very small amount of F incorporation. [00087] Anti-wear and friction reducing performance of different chain length diesters from C6 to C14 was compared. All of these non-symmetric, partially fluorinated diesters imparted some benefits, with the longer chain diacids giving the greater benefits. Therefore, the preferred number of carbon atoms in the backbone is 9 or more or the wear scar by the BOCLE test as described herein is less than about 0.75 when the additive is present at about 0.2% fluorine.

The synthetic route of 112-70-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; E. I. du Pont de Nemours and Company; US6734320; (2004); B2;,
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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. 6966-10-5, name is (3,4-Dimethylphenyl)methanol, molecular formula is C9H12O, 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. Product Details of 6966-10-5

General procedure: To a solution of phenylmethanols 5a-w (5 mmol) dissolved in methylene chloride (50 mL) in an ice-water bath was added phosphorus tribromide (5.5 mmol), and the mixture was stirred at the same temperature for 30 min. The mixture was washed with cool water, dried over anhydrous Na2SO4 and concentrated under reduced pressure to yield (bromomethyl)benzenes 6aew as offwhite solids or light yellow oils

With the rapid development of chemical substances, we look forward to future research findings about 6966-10-5.

Reference:
Article; Feng, Lianshun; Lv, Kai; Liu, Mingliang; Wang, Shuo; Zhao, Jing; You, Xuefu; Li, Sujie; Cao, Jue; Guo, Huiyuan; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 125 – 136;,
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Related Products of 2516-33-8, 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 2516-33-8, name is Cyclopropylmethanol. This compound has unique chemical properties. The synthetic route is as follows.

To a stirred solution of cyclopropanemethanol (1.00 g, 0.90 mL, 13.87 mmol) and pyridine (1.43 g, 1.45 mL, 18.03 mmol) in acetonitrile (80 mL) was added N,N’-disuccinimidyl carbonate (4.62 g, 18.03 mmol) in one portion and the solution was heated to 40 C. for 4 h. After cooling to room temperature, the solvent was evaporated to dryness and the residue was taken up in dichloromethane (150 mL), washed with saturated aqueous sodium bicarbonate (2×150 mL) and saturated brine (100 mL), dried (MgSO4) and concentrated to afford cyclopropanemethanol-(CO.N-hydroxysuccinimide) (2.93 g, 99%), as a colourless oil that was used without further purification.

According to the analysis of related databases, 2516-33-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SHIRE LLC; US2012/65152; (2012); A1;,
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Application of 17701-61-0, Adding some certain compound to certain chemical reactions, such as: 17701-61-0, name is Benzyl 3-hydroxy-2,2-dimethylpropanoate,molecular formula is C12H16O3, 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 17701-61-0.

(a) To a solution of 4-isopropyl-6-hydroxy-2-(1-phenyl-3-trifluoromethylpyrazol-5-yl-oxymethyl)-1,2-benzisothiazol-3(2H)-one 1,1-dioxide (1 g; 2.08 mmol) in THF containing (Ph)3 P (550 mg; 2.09 mmol) and DEAD (360 mg; 2.07 mmol) was added benzyl 2,2-dimethyl-3-hydroxypropionate (440 mg;2.099 mmol) and the resulting mixture was stirred at room temperature for 15 hours. The mixture was concentrated in vacuo and the residue was purified by flash chromatography (silica gel) to afford 440 mg (32%) of 4-isopropyl-6-[2-(phenylmethyloxycarbonyl-2-methyl)propoxy]-2-(1-phenyl-3-trifluoromethylpyrazol-5-yl-oxymethyl)-1,2-benzisothiazol-3(2H)-one 1,1-dioxide (Formula I: R1 =Ph; R2 =CF3; R3 =H; R4 =CH(CH3)2; R5 =6-OCH2 C(CH3)2 CO2 CH2 Ph) as a gum.

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. 17701-61-0, Benzyl 3-hydroxy-2,2-dimethylpropanoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sanofi; US5750550; (1998); A;,
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Synthetic Route of 33420-52-9 ,Some common heterocyclic compound, 33420-52-9, molecular formula is C3H6F2O, 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 tert-butyl 4-(1-(4-(methoxycarbonyl)-3-methylthiophen-2-yl)propylidene)piperidine-1-carboxylate (12.1 g, 31.9 mmol) was added HC1 in dioxane (30 mL, 120 mmol). After stirring for 30 min the reaction was evaporated to dryness to give the crude amine hydrochloride salt as a white solid foam. To a stirred solution of 2,2-difluoropropan-l-ol (16.3 g, 170 mmol) and pyridine (16.3 mL, 202 mmol) in CH3CN (250 mL) at 0 C in an ice bath was added dropwise Tf20 (28 mL, 166 mmol). The reaction was stirred for 30 min at 0 C, then added cold to a slurry of the above amine hydrochloride and K2C03 (46.8 g, 339 mmol) in CH3CN (100 mL). The reaction was rinsed down with CH3CN (50 mL). The reaction was allowed to warm to RT, heated to 50 C and stirred for 6 h. The reaction was evaporated to dryness under vacuum, taken up in DCM, washed with water, brine, dried (Na2S04), filtered, and concentrated under vacuum. The residue was purified by silica gel chromatography (Isco RediSep Rf Gold 120g, 5 to 15% EtOAc in hexanes). The pure fractions were combined and evaporated to dryness under vacuum to give methyl 5-(1-(1-(2,2- difluoropropyl)piperidin-4-ylidene)propyl)-4-methylthiophene-3 -carboxylate ( 10.05 g, 24.74 mmol, 78 % yield) as a colorless oil. 1H NMR (400 MHz, CDCl3) delta 8.03 (s, 1H), 3.86 (s, 3H), 2.70 (t, J=12.6 Hz, 4H), 2.57 – 2.43 (m, 4H), 2.32 (br. s., 2H), 2.25 (s, 3H), 2.06 (br. s., 2H), 1.67 (t, J=18.8 Hz, 3H), 0.94 (t, J=7.5 Hz, 3H). MS(ES) [M+H]+ 358.2.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,33420-52-9, its application will become more common.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; KNIGHT, Steven David; NEWLANDER, Kenneth Allen; TIAN, Xinrong; (112 pag.)WO2016/66697; (2016); A1;,
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Adding a certain compound to certain chemical reactions, such as: 145691-59-4, (3,5-Dibromophenyl)methanol, 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, Safety of (3,5-Dibromophenyl)methanol, blongs to alcohols-buliding-blocks compound. Safety of (3,5-Dibromophenyl)methanol

3, [5-DIBROMOBENZYL ALCOHOL] (9.8 g, 36.9 [MMOL)] is dissolved in DMF (100 ml) and, while stirring, thionyl chloride (5 [ML)] is slowly added dropwise. [AFTER30 M IN,] the reaction mixture is concentrated in vacuo and the residue is taken up in EA (150 [ML). FORWORKUP,] the organic phase is washed with ice-water (50 ml) and then with half-saturated aqueous NaCi solution (50 [ML).] The organic phase is dried over [MGS04,] filtered and concentrated in vacuo. The title compound (10.4 g) is obtained as a yellow solid. TLC [PE/EA (95: [05)], RF=] 0.69.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,145691-59-4, (3,5-Dibromophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; ALTANA PHARMA AG; WO2004/12731; (2004); A1;,
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Reference of 623-04-1, Adding some certain compound to certain chemical reactions, such as: 623-04-1, name is (4-Aminophenyl)methanol,molecular formula is C7H9NO, 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 623-04-1.

For Fmoc-Leu-PABA 2j, a solution of Fmoc-Leu-OH (353 mg, 1 mmol), EEDQ (495 mg, 2 mmol) and PABA (222 mg, 1.8 mmol) in DCM (10 ml) was stirred for 10 h. All volatiles were removed on a rotovap, the residue was dissolved in Et2O (40 ml), chilled on dry ice for 2h and the solid was separated by centrifugation. The obtained crude material was purified on a column, eluent gradient of MeOH (1-2%) in CHCl3. Yield 444 mg (97%). MS: 459.4 [M+1]+.

According to the analysis of related databases, 623-04-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ARROWHEAD RESEARCH CORPORATION; CHENG, Weijun; WONG, So; ALMEIDA, Aaron, M.; ROZEMA, David, B.; BLOKHIN, Andrei, V.; CARLSON, Jeffrey, C.; WO2015/21092; (2015); A1;,
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Application of 5182-44-5, 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.5182-44-5, name is 2-(3-Chlorophenyl)ethanol, molecular formula is C8H9ClO, molecular weight is 156.6095, as common compound, the synthetic route is as follows.

In a flame-dried 250 mL round-bottom flask equipped with an argon line, the appropriate alcohol (21a-26a) (1 eq. ) was placed and was dissolved in ether/acetonitrile (3: 1). To this solution, triphenylphosphine (3 eq. ), imidazole (3 eq. ) and iodine (3 eq.) were added in this order. The reaction mixture was kept at room temperature for 1 hours and monitored by TLC. The reaction mixture was filtered and washed with ether. The organic layers were then washed with brine, dried over MgS04, filtered and concentrated in vacuo. The residue was purified via flash chromatography on silica gel eluting with 1% ethyl acetate/hexanes to give 21b-26b in 58-88% yield. m-Chlorophenethyl iodine (21b) H NMR (CDC13) : 8 7.21-7. 19 (q, 3H), 7.12 (t, 1H), 3.52 (t, 2H), 3.28 (t, 2H).’3CNMR (CDC13) : 8 140.90, 134.14, 129.69, 129.06, 127.02, 126.45, 38.69, 11,27. IR (liquid film) 2948,2879, 1598,1574, 1429 FT-ICRMS : m/z 267. 52 (M. +H).

The chemical industry reduces the impact on the environment during synthesis 5182-44-5, I believe this compound will play a more active role in future production and life.

Reference:
Patent; UNIVERSITY OF MISSISSIPI; WO2003/95444; (2003); A1;,
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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. 19819-98-8, name is 2-(o-Tolyl)ethanol, molecular formula is C9H12O, 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. Application In Synthesis of 2-(o-Tolyl)ethanol

General procedure: To a 1 dram vial equipped with a stir bar was added the alcohol (0.080 mmol), isopropyl (S)-2-(tert-butoxy)-2-(4?-(4,4-dimethylpiperidin- 1 -yl)-5-hydroxy-6?-methyl- [2,3?-bipyridinj-5?-yl)acetate (25 mg, 0.053 mmol), and triphenylphosphine (20.9 mg, 0.080 mmol) as a solution in THF (0.25 mL). To the solution was added DIAD (0.016 mL, 0.080 mmol) as a solution in THF (0.25 mL). The solution was stirred at r.t. for 30mm to 18 h. The reaction solution was concentrated under a N2 stream. The residue wasdissolved in EtOH (1.0 mL). To the solution was added aq. NaOH (5.0 M, 0.110 mL,0.532 mmol). The vial was capped, then placed in a 85 C heating block with stirring for4 h to 18 h. The mixture was cooled to r.t., then was filtered through a 0.4 micron syringefilter and the filtrate was directly subjected to HPLC purification to afford the purifiedproduct.

With the rapid development of chemical substances, we look forward to future research findings about 19819-98-8.

Reference:
Patent; VIIV HEALTHCARE UK (NO.5) LIMITED; BELEMA, Makonen; BOWSHER, Michael S.; DESKUS, Jeffrey A; EASTMAN, Kyle J.; GILLIS, Eric P; FRENNESSON, David B; IWUAGWU, Christiana; KADOW, John F.; NAIDU, B. Narasimhulu; PARCELLA, Kyle E.; PEESE, Kevin M; SAULNIER, Mark G; SIVAPRAKASAM, Prasanna; (463 pag.)WO2018/127800; (2018); A1;,
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Application of 27489-62-9 ,Some common heterocyclic compound, 27489-62-9, molecular formula is C6H13NO, 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 6-chloro-3-(7-methoxythieno[3,2-c]pyridin-2-yl)imidazo[1,2-b]pyridazine (20 mg, 0.0631 mmol, 1.0 equiv) in DMSO (2.0 mL) was added p-toluene sulfonic acid monohydrate (12 mg, 0.0631 mmol, 1.0 equiv) and amine (36 mg, 0.316 mmol, 5.0 equiv) and heated to 100 C. for 24 h. The reaction mixture was diluted with water and extracted with ethyl acetate. Purification by column chromatography using 5% methanol in dichloromethane elution gave 20 mg of the yellow solid, 80%. [0598] Compound 213, 217 was physically characterized by electrospray ionization mass spectrometry. Structures and molecular masses are given below in Table 59.

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. 27489-62-9, trans-4-Aminocyclohexanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Califia Bio, Inc.; GOODFELLOW, VAL S.; NGUYEN, THONG X.; RAVULA, SATHEESH B.; GELBARD, HARRIS A.; US2014/256733; (2014); A1;,
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