Month: September 2021

Adding a certain compound to certain chemical reactions, such as: 67853-03-6, Methyl 3-(hydroxymethyl)benzoate, 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, Quality Control of Methyl 3-(hydroxymethyl)benzoate, blongs to alcohols-buliding-blocks compound. Quality Control of Methyl 3-(hydroxymethyl)benzoate

Entry 27 Boron trifluoride etherate (25 muL, 0.20 mmol, 0.2 eq.) was added dropwise at -20C under argon to a stirred solution of 2,3,4,6-tetra-O-acetyl-alpha-d-galactopyranosyl trichloroacetimidate (1c) (500 mg, 1.01 mmol, 1 eq.) and methyl 3-hydroxymethylbenzoate (2d) (503 mg, 3.03 mmol, 3 eq.) in freshly distilled CH2Cl2 (8 mL). After 1 hour, Et3N (0.2 mL) was injected into the reaction mixture. Then, the solvent was evaporated, the residue was purified by silica gel column chromatography (PE:EtOAc, 5:1 to 3:1) to afford (1-methoxycarbonylphen-3-yl)methyl 2,3,4,6-tetra-O-acetyl-beta-d-galactoside (3e) as a white foam (397 mg, 79%). Rf = 0.27 (PE:EtOAc = 2:1); [alpha]D20 = -31.8 (c = 0.4, CH2Cl2); 1H NMR (400 MHz, CDCl3), delta (ppm): 7.94 (m, 2H, 2 HAr), 7.46 (d, J = 7.6 Hz, 1H, HAr), 7.40 (t, J = 8.0 Hz, 1H, HAr), 5.36 (d, J = 2.9 Hz, 1H, H4), 5.26 (dd, J = 10.4, 8.0 Hz, 1H, H2), 4.97 (dd, J = 10.5, 3.4 Hz, 1H, H3), 4.91 (d, J = 12.6 Hz, 1H, OCH2a), 4.65 (d, J = 12.6 Hz, 1H, OCH2b), 4.51 (d, J = 8.0 Hz, 1H, H1), 4.21-4.06 (m, 2H, H6), 3.91-3.85 (m, 4H, OMe, H5), 2.13 (s, 3H, COCH3), 2.03 (s, 3H, COCH3), 2.03 (s, 3H, COCH3), 1.95 (s, 3H, COCH3); 13C NMR (100 MHz, CDCl3), delta (ppm): 170.5 (C=O), 170.3 (C=O), 170.2 (C=O), 169.6 (C=O), 166.8 (COOMe), 137.3 (CAr), 132.2 (CAr-H), 130.4 (CAr), 129.2 (CAr-H), 128.70 (CAr-H), 128.65 (CAr-H), 100.0 (C1), 70.9 (C3), 70.8 (C5), 70.1 (OCH2), 68.8 (C2), 67.1 (C4), 61.3 (C6), 52.2 (OMe), 20.7 (3 × COCH3), 20.6 (COCH3); HRMS m/z: calcd. for C23H28NaO12, [M+Na]+ 519.1473, found 519.1466.

The synthetic route of 67853-03-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Wang, Shuai; Lafont, Dominique; Rahkila, Jani; Picod, Benjamin; Leino, Reko; Vidal, Sebastien; Carbohydrate Research; vol. 372; (2013); p. 35 – 46;,
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Reference of 2002-24-6, Adding some certain compound to certain chemical reactions, such as: 2002-24-6, name is 2-Aminoethanol hydrochloride,molecular formula is C2H8ClNO, 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 2002-24-6.

1-Nitro-9-Hydroxyethylaminoacridine This compound is synthesised generally using the methods described in EP 38579. Specifically, 2 g of 2-amino-ethanol hydrochloride is added to 6.4 g of 1-nitro-9-phenoxyacridine dissolved in 20 g of freshly distilled phenol. The mixture is heated for 40 minutes at a temperature of 80 C. and then cooled, diluted with ether. It is then poured into dry ether that was acidified with an ethereal solution of hydrogen chloride. The orange colored precipitate of 1-nitro-9-(2-hydroxyethylamino)-acridine hydrochloride, obtained in this way is filtered and crystallized from dry ethanol. The melting point of the compounds obtained was 170 C., with decomposition. Yield 91%. Elementary analysis for the formula: C15H14N3O3Cl:calculated:56.47%; C, 4.42%; H, 13.17%; N. determined: 56.44%; C, 4.40%; H, 13.03%; N.

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. 2002-24-6, 2-Aminoethanol hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Tiwari, Raj; Miller, Daniel G.; Konopa, Jerzy Kazimierz; Wysocka-Skrzela, Barbara; US2002/37831; (2002); A1;,
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Reference of 3973-18-0, Adding some certain compound to certain chemical reactions, such as: 3973-18-0, name is Propynol ethoxylate,molecular formula is C5H8O2, 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 3973-18-0.

General procedure: Alkynes 16 or 11a-11d (6mmol) were added to a solution of salinomycin azido derivative 15 (10mmol), Na ascorbate (1mmol), and copper sulphate (3mmol) in tert-butanol (5mL) at 4C, followed by adding water (5mmol), and stirring continuously for 24hat 55C. Then, the reaction was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous Na2SO4, filtered, and concentrated in vacuum. The product was purified by flash chromatography to give 1,2,3-triazole derivatives 3a-3g and 4a-4d.

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. 3973-18-0, Propynol ethoxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Huang, Minjian; Deng, Zixin; Tian, Jian; Liu, Tiangang; European Journal of Medicinal Chemistry; vol. 127; (2017); p. 900 – 908;,
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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 186602-93-7, name is (2-Amino-4-(trifluoromethyl)phenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. Product Details of 186602-93-7

5.1.105 6,7-Didehydro-17-methyl-7′-trifluoromethylquinolino[2′,3′:6,7]morphinan-3,14beta-diol hydrochloride (SYK-72) SYK-72 was prepared from compound 28c according to the procedure used to prepare SYK-27. Yield, 73%; a white amorphous solid. Mp 233-234 C (dec). Anal. Calcd for C25H23F3N2O2·1.0HCl·0.8H2O: C, 61.11; H, 5.25; N, 5.70. Found: C, 61.11; H, 5.36; N, 5.83.

With the rapid development of chemical substances, we look forward to future research findings about 186602-93-7.

Reference:
Article; Ida, Yoshihiro; Matsubara, Ayaka; Nemoto, Toru; Saito, Manabu; Hirayama, Shigeto; Fujii, Hideaki; Nagase, Hiroshi; Bioorganic and Medicinal Chemistry; vol. 20; 19; (2012); p. 5810 – 5831;,
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Adding a certain compound to certain chemical reactions, such as: 455-01-6, 2-(3-(Trifluoromethyl)phenyl)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, HPLC of Formula: C9H9F3O, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C9H9F3O

General procedure: To a stirred solution of betulonic acid (3, 0.883 g, 1.94 mmol) in anhydrous CH2Cl2 (10 mL) was added oxylchoride (1.70 mL,19.45 mmol) at rt and kept for 2 h. The solvent was removed under vaccum, and another 3 mL CH2Cl2 was added to the residue and then removed again. To the residue was added anhydrous CH2Cl2 (8 mL), 2-cyclopropylethanol (0.5025 g, 5.83 mmol) and triethyl amine (2.71mL, 19.44 mmol), and the mixture was stirred for 24 h at rt. After removal of solvent under vaccumn, the residue was purified by silica gel column chromatography (hexane/EtOAcas eluent) to provide desired compound 10 (760 mg). White solid, yield 75%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,455-01-6, 2-(3-(Trifluoromethyl)phenyl)ethanol, and friends who are interested can also refer to it.

Reference:
Article; Li, Jizhen; Goto, Masuo; Yang, Xiaoming; Morris-Natschke, Susan L.; Huang, Li; Chen, Chin-Ho; Lee, Kuo-Hsiung; Bioorganic and Medicinal Chemistry Letters; vol. 26; 1; (2016); p. 68 – 71;,
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Related Products of 83647-43-2, 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 83647-43-2 as follows.

Step B. The intermediate from Step A above (18.1 g) was dissolved in anhydrous CH2Cl2 (150 mL) under nitrogen and the reaction vessel was cooled to 00C in an ice bath. To this cooled solution was added PBr3 (5.52 mL) over a 10 min period. Once the addition was complete, the reaction mixture was warmed to room temperature and stirred for an additional 12 h. The mixture was cooled in an ice bath and quenched by the dropwise addition of MeOH (20 mL). The organic phase was washed with saturated NaHCO3 (2 x 150 mL), dried over anhydrous MgSO4, filtered, and then concentrated to afford the intermediate (23.8 g; 97 %) as viscous oil. 1H-NMR (CDCl3) delta = 2.50 (s, 3 H), 4.50 (s, 2 H), 7.00 (t, H), 7.25 (d, 1 H), 7.50 (d, 1 H). Step B. Under a nitrogen atmosphere PBr3 (5.52 mL) was added over a lO min period to an ice cooled solution of the title compound from Step A above (18.1 g) in anhydrous CH2Cl2 (15O mL). The cooling bath was removed and mixture stirred at room temperature for 12 h. The mixture was cooled (0-5C), quenched by dropwise addition of MeOH (20 mL), washed with saturated aqueous NaHCO3 (2 x 15O mL), dried (MgSO4), filtered and concentrated to afford the title compound as a viscous oil (23.8 g, 97%). 1H-NMR (CDCl3) delta = 7.50 (d, 1 H), 7.25 (d, 1 H), 7.00 (t, 1 H), 4.50 (s, 2 H), 2.50 (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,83647-43-2, its application will become more common.

Reference:
Patent; ALANTOS PHARMACEUTICALS HOLDING, INC.; WO2008/63671; (2008); A2;,
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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. 25574-11-2, name is 3-(4-Bromophenyl)propan-1-ol, the common compound, a new synthetic route is introduced below. HPLC of Formula: C9H11BrO

(41-3) Synthesis of 4-bromo-1-(3-bromopropyl)benzene (compound 41-3) Compound 41-2 (3.63 g) was dissolved in methylene chloride (40 ml), triphenylphosphine (4.88 g) and N-bromosuccinimide (3.31 g) were added under ice-cooling, and the mixture was stirred under ice-cooling for 2 hr, and at room temperature for 4 hr. The reaction mixture was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. Diethyl ether (100 ml) was added, and the precipitated triphenylphosphine oxide was filtered off. The concentrate of the filtrate was purified by silica gel column chromatography (hexane alone) to give the object product (1.87 g) as a colorless oil. 1H-NMR(CDCl3) delta (ppm): 2.10-2.17(2H, m), 2.74(2H, t, J=7.4Hz), 3.38(2H, t, J=6.5Hz), 7.08(2H, d, J=8.3Hz), 7.41(2H, dd, J=8.3, 1.9Hz).

The synthetic route of 25574-11-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Mitsubishi Tanabe Pharma Corporation; EP2168944; (2010); A1;,
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Electric Literature of 616-29-5, 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. 616-29-5, name is 1,3-Diaminopropan-2-ol. A new synthetic method of this compound is introduced below.

Example 2 To 13.5 g (0.15 mol) of 1,3-diaminopropan-2-ol and 14.4 g (0.36mol) of NaOH in 400 ml THF and 200 ml H2O at 0 C. was added 72 g (0.33 mol) of Boc2O in portions. The reaction mixture was warmed up to RT and stirred overnight. To this mixture was added 300 ml of EtOAc. The layers were separated and the aqueous layer was extracted with 200 ml EtOAc. The combined organic layer was dried with MgSO4 and concentrated to give di-tert-butyl 2-hydroxypropane-1,3-diyldicarbamate in quantitative yield.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,616-29-5, 1,3-Diaminopropan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; Morgan, Bradley P.; Muci, Alex; Kraynack, Erica; Lu, Pu-Ping; Tochimoto, Todd; Morgans, David J.; US2007/66626; (2007); A1;,
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Electric Literature of 1875-88-3 , The common heterocyclic compound, 1875-88-3, name is 2-(4-Chlorophenyl)ethanol, molecular formula is C8H9ClO, 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.

The present invention uses SM-A and LCS-1 condensation to prepare Impurity F.Specific operations are as follows: 40g of p-chlorophenylacetic acid was added to 400ml of tetrahydrofuran,Stirring at room temperature dissolved; lithium aluminum hydride in batches, temperature control at 25 ~ 30 ,After the reaction was stirred for 20 hours, 200 ml of water was added slowly and the addition was completed.Add ethyl acetate 400ml stirred 30min, liquid separation, organic phase plus 200ml saturated brine and dried over 20g anhydrous sodium sulfate, filtered, the filtrate was concentrated under reduced pressure 40 ~ 45 ,36.7 g of oil (S2) was obtained; S2 was added to the reaction flask, the temperature was lowered to 0 to 5 C in ice water,Slowly dropping phosphorus tribromide, dropping temperature during the course of 0 ~ 5 , the dropwise addition is completed,Heated to 25 ~ 30 , incubated for 3h,Add water 80ml, stirred 30min, liquid separation, the aqueous phase was extracted with dichloromethane 100ml × 2,The organic phases were combined and concentrated under reduced pressure to give an oil (S3): 48.8 g. Yield: 94.9%.

The synthetic route of 1875-88-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shandong Kexing Biological Products Co., Ltd.; Cui Ning; Dong Xiangjun; Hao Zhihai; (34 pag.)CN106478506; (2017); A;,
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Reference of 495-76-1, Adding some certain compound to certain chemical reactions, such as: 495-76-1, name is Benzo[d][1,3]dioxol-5-ylmethanol,molecular formula is C8H8O3, 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 495-76-1.

Dissolve 5.8 ml (0.06 mol) of phosphorus tribromide in 20 ml of ether and slowly instill 7.1 g (0.05 mol)In a solution of 3,4-dioxymethylenebenzaldehyde in ether, the reaction was stirred at 0C for 3 hours. After stopping the reaction,Saturated sodium carbonate solution was quenched, and the mixture was partitioned and washed with saturated saline water and dried over anhydrous sodium sulfate for 8 hours.The desiccant was filtered off and the solvent was evaporated under reduced pressure to give 8.9 g of a pale yellow liquid of Vb in a yield of 83.7%.

According to the analysis of related databases, 495-76-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; The Chinese People’s Liberation Army Military Academy Of Medical Sciences Poison Pharmaceutical Institute; Zhong Bohua; Zhang Ping; He Xinhua; Shi Weiguo; Fan Shiyong; Yao Yishan; Jia Hongxin; (20 pag.)CN103804341; (2018); B;,
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