Month: June 2021

Electric Literature of 162744-59-4, 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.162744-59-4, name is (4-Bromo-2,6-difluorophenyl)methanol, molecular formula is C7H5BrF2O, molecular weight is 223.0148, as common compound, the synthetic route is as follows.

To a solution of (4-bromo-2,6-difluorophenyl)methanol (2 g, 8.97 mmol) in DCM (80 inL) was added tribromophosphine (2.91 g, 10.76 mmol) at 0 C. The resulting mixture was stirred at rt. After LCMS analysis showed the starting material had disappeared, the mixture was washed with aqueous NaHC03 (40 inL) and brine (30 mL). The organic layer was dried over NaaSOzi, filtered and concentrated. The crude material was purified by silica column chromatography (PE/EA = 5/1) to yield a colorless oil of 5-bromo-2-(bromomethyl)-l,3-difluorobenzene (1.6 g, 5.48 mmol, 61.2% yield): lH NMR (400 MHz, CD3OD) delta 7.12 (d, J= 6.8 Hz, 2H), 4.47 (s, 2H).

The chemical industry reduces the impact on the environment during synthesis 162744-59-4, I believe this compound will play a more active role in future production and life.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; EIDAM, Hilary Schenck; DEMARTINO, Michael P.; GONG, Zhen; GUAN, Amy Huiping; RAHA, Kaushik; WU, Chengde; YANG, Haiying; YU, Haiyu; ZHANG, Zhiliu; CHEUNG, Mui; WO2014/141187; (2014); A1;,
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Synthetic Route of 617-94-7, Adding some certain compound to certain chemical reactions, such as: 617-94-7, name is 2-Phenyl-2-propanol,molecular formula is C9H12O, 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 617-94-7.

EXAMPLE 27 N-((lR,2S)-2-((S)-4-(4-Chlorophenyl)-4-hydroxy-3,3-dimethylpiperidine-l- carbonyl)cyclohexyl)-c/s-3,4-dihydroxycyclopentanecarboxamideStep 1: 2-Phenylpropan-2-yl 2,2,2-trichloroacetimidate [00167] A suspension of 60% sodium hydride in mineral oil (0.42 g, 10.50 mmol) in diethyl ether (10 mL) was treated with the dropwise addition of a solution of 2- phenylpropan-2-ol (12.02 mL, 86 mmol) in diethyl ether (30 mL). Upon completion of addition, the mixture was stirred for 30 minutes, during which time a nearly clear solution was observed. After this time, the mixture was cooled to 0 0C and then treated with the dropwise addition of trichloroacetonitrile (8.18 mL, 82 mmol), which caused the mixture to turn dark brown. The reaction was allowed to warm to room temperature over 1 hour, and then was concentrated in vacuo to yield a residue. The residue was dissolved in hexanes (10 mL) and treated with methanol (0.424 mL, 10.48 mmol), and the resulting mixture was stirred vigorously for 5 minutes. The resulting black suspension was filtered through glass fiberglass filter paper, and the collected solids were rinsed 3X with hexanes. The combined filtrates were concentrated in vacuo to yield 2-phenylpropan-2-yl 2,2,2-trichloroacetimidate (23.8 g, 85 mmol, 99 % yield) as an amber oil which was used as-is in the next step.

According to the analysis of related databases, 617-94-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2009/15166; (2009); A1;,
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Reference of 3513-81-3, 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 3513-81-3, name is 2-Methylenepropane-1,3-diol. This compound has unique chemical properties. The synthetic route is as follows.

Step A Synthesis of Compound Int-19a TBDPSC1 (9.0 mL, 35.0 mmol) was added dropwise to a stirred hazy solution of 2- methylenepropane-l,3-diol (3 g, 34.1 mmol) and imidazole (4.70 g, 69.0 mmol) in DCM (340 mL). The reaction mixture was stirred at room temperature overnight. The following morning, the reaction mixture was concentrated under reduced pressure (~80 mL) before being filtered through a pad of celite, rinsing over with additional DCM / MeOH. The filtrate was evaporated under reduced pressure. The resulting oil was purified by silica gel column (220 g) (0452) chromatography eluting with 0-20% EtOAc / hexanes to afford compound Int-19a. NMR (500 MHz, CDCb): d 7.69 (d, J = 7.4 Hz, 4H); 7.49 – 7.37 (m, 6H); 5.16 (app. s, 1H); 5.13 (app. s, 1H); 4.27 (s, 2H); 4.19 (d, J = 6.2 Hz, 2H); 1.80 (t, J = 6.1 Hz, 1H); 1.08 (s, 9H).

According to the analysis of related databases, 3513-81-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK SHARP & DOHME CORP.; YU, Tao; APGAR, James, M.; WHITEHEAD, Alan; ZHANG, Yonglian; HU, Zhiyong; SHURTLEFF, Valerie, W.; MCCAULEY, John, A.; RAHEEM, Izzat, T.; (97 pag.)WO2019/209667; (2019); A1;,
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Electric Literature of 122763-67-1, Adding some certain compound to certain chemical reactions, such as: 122763-67-1, name is tert-Butyl 3-hydroxypent-4-enoate,molecular formula is C9H16O3, 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 122763-67-1.

[0216] To a solution of tert-butyl 3-hydroxypent-4-enoate, XL VI (674 mg, 3.92 mmol) in DCM (15 mL) was added diisopropylallylboronate XLV(2 g, 11.76 mmol) via syringe. To the mixture was then added Grubbs’ first generation catalyst (260 mg, 0.31 mmol, 7.5 mol%) and the vessel was purged with argon. The reaction was heated at 65 C under nitrogen for 18h. The mixture was concentrated under vacuum and the residue was purified by flash column chromatography (100% hexane?30% EtOAc/hexane) to afford tert-butyl 2-(2- hydroxy-3,6-dihydro-2H-l,2-oxaborinin-6-yl)acetate XL VII (770 mg, 3.63 mmol, 92.7% yield).

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. 122763-67-1, tert-Butyl 3-hydroxypent-4-enoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; REMPEX PHARMACEUTICALS, INC.; DUDLEY, Michael, N.; HECKER, Scott; RODNY, Olga; WO2013/122888; (2013); A2;,
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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.115-20-8, name is Trichloroethanol, molecular formula is C2H3Cl3O, molecular weight is 149.4, as common compound, the synthetic route is as follows.SDS of cas: 115-20-8

A mixture of CLTAM (1.0 g, 2.59 mmol) and K2C03 (0.39 g, 2.85 mmol) in 2.2,2-trichloroethanol (5 mL) was stirred at room temperature for 16 hours. Water (70 mL) was added, then product was extracted to MeTHF (3 x 20 mL), combined organic layers ware dried over MgS04, and then concentrated to afford crude product, which was purified by chromatography (Si02, hexane:EtOAc) to afford title compound as white powder (1.00 g, 78% yield). MP 1 18C; MS (ESI) mlz: 498 [MH]

At the same time, in my other blogs, there are other synthetic methods of this type of compound,115-20-8, Trichloroethanol, and friends who are interested can also refer to it.

Reference:
Patent; LEK PHARMACEUTICALS D.D.; ZUPANCIC, Borut; MARAS, Nenad; STERK, Damjan; WO2013/60837; (2013); A1;,
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Application of 2503-56-2 ,Some common heterocyclic compound, 2503-56-2, molecular formula is C6H6N4O, 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.

[0171] Compounds 4c. 5-Methyl-pyrazolo[l,5-alpha]pyrimidin-7-ol/7-Methyl-imidazo[l,2- alpha]pyrimidin-5-ol/5-Methyl-[l,2,4]triazolo[l,5-alpha]-pyrimidin-7-ol (3c) (6.5 mmol) was added to 1.82 ml (19.5 mmol) of phosphorus oxychloride and heated under reflux for 30-60 minutes, in a round bottom flask, during which time the solid dissolved and hydrogen chloride was evolved. Excess phosphorus oxychloride was removed by distillation at reduced pressure on a steam-bath and the residue triturated with ice water. Product was extracted from the aqueous mixture with methylene chloride, evaporated and purified by column chromatography using 60% EtOAc/Hexane at a yield of 42-70%.[0172] 7-Chloro-5-methyl-[l,2,4]triazolo[l,5-alpha]pyrimidine (4c). mp. 150 0C. 1H NMR (300 MHz, CDCl3): delta 8.50 (s, IH), 7.15 (s, IH), 2.75 (s, 3H). MS mlz 169.1 (M + H+).

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. 2503-56-2, 7-Hydroxy-5-methyl-1,3,4-triazaindolizine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOARD OF REGENTS, UNIVERSITY OF TEXAS SYSTEM; UNIVERSITY OF WASHINGTON; WO2009/82691; (2009); 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 115-20-8, name is Trichloroethanol. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 115-20-8

1. t-BOC-L-Alanine 2,2,2-Trichloroethyl Ester t-BOC-L-Alanine was treated with N,N’-carbonyldiimidazole in DMF followed by 2,2,2-trichloroethanol. After the reaction was complete the solvent was removed, the residue dissolved in EtOAc and the EtOAc layer washed with water, dilute hydrochloric acid and 5% sodium bicarbonate. The EtOAc layer was dried with magnesium sulfate then evaporated to give the product.

With the rapid development of chemical substances, we look forward to future research findings about 115-20-8.

Reference:
Patent; Mallinckrodt, Inc.; US4406832; (1983); A;,
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Electric Literature of 2615-15-8, 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.2615-15-8, name is 3,6,9,12,15-Pentaoxaheptadecane-1,17-diol, molecular formula is C12H26O7, molecular weight is 282.33, as common compound, the synthetic route is as follows.

j00346j A solution of 3,6,9,12,15-pentaoxaheptadecane-1,17-diol (5 g, 1.70 mmol) in THF (100 mL) was charged with tosyl chloride (10.1 g, 5.30 mmol) and solution of potassium hydroxide (5.9 g, 5.30 mmol) in H20 (100 mL) at room temperature. The resulting solution was heated to 60 C for 5 h then cooled to room temperature and evaporated in vacuo. Theresidue obtained was diluted with DCM (100 mL) and filtered. The filtrate was concentrated in vacuo resulting in a crude compound which was purified by chromatography on silica gel, eluting with 1-3% methanol in DCM to obtain 8 g, 76% yield of the title compound as colorless oil. ?H NMR (400 MHz, DMSO-d6): oe = 7.78 (d, J= 7.94 Hz, 4H), 7.48 (d, J= 8.38 Hz, 4H), 4.08-4.13 (m, 4H), 3.54-3.59 (m, 4H), 3.43 -3.50 (m, 16H), 2.42 (s, 6H).

Statistics shows that 2615-15-8 is playing an increasingly important role. we look forward to future research findings about 3,6,9,12,15-Pentaoxaheptadecane-1,17-diol.

Reference:
Patent; COFERON, INC.; FOREMAN, Kenneth, W.; JIN, Meizhong; WANNER, Jutta; WERNER, Douglas, S.; WO2015/106292; (2015); A1;,
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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. 186020-66-6, name is tert-Butyl 12-Hydroxy-4,7,10-trioxadodecanoate. This compound has unique chemical properties. The synthetic route is as follows. Quality Control of tert-Butyl 12-Hydroxy-4,7,10-trioxadodecanoate

Step b: The crude product from step a (40.23 g, 0.157 mol) was dissolved in 50 mL pyridine, cooled to 0 C., and Ts-Cl (32.92 g, 0.173 mol) was added slowly. The flask containing the reaction mixture was sealed and placed in a refrigerator at 0 C. for 24 h. The reaction mixture was poured into ice/H2O, and the aqueous layer was extracted with CH2Cl2 (3×100 mL). The combined organic layers were washed with 2% HOAc in H2O, and dried over anhydrous MgSO4. The solvent was removed under vacuum to yield the tosylate as colorless oil. The oil was dried under vacuum (52.97 g, mol, 78%). HPLC: tR=13.0 min.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 186020-66-6, tert-Butyl 12-Hydroxy-4,7,10-trioxadodecanoate.

Reference:
Patent; Wilbur, D. Scott; Pathare, Pradip M.; Hamlin, Donald K.; Wan, Feng; US2006/228325; (2006); A1;,
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Reference of 53463-68-6, 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. 53463-68-6, name is 10-Bromodecanol, molecular formula is C10H21BrO, 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.

10-Bromodecan-1-ol (0.24 g, 1.0 mmol) in dry THF (1mL) was mixed with 3,4-dihydro-2H-pyran (0.11 g, 1.25 mmol) and iodine (0,05 g, 0.2 mmol). The mixture was added to a 50 mL conical flask, and a small funnel was placed over it to reduce possible evaporation of solvent. The flask was irradiated in microwave oven at 600 MW power for 3min. On cooling, the reaction mixture was diluted with chloroform (30 mL) and washed with 10percent aq. sodium thiosulphate solution (2 x 5 mL), water (2 x 5 mL), brine and dried. Evaporation of the solvent under reduced pressure and purification by silica gel column chromatography (1:9 ethyl acetate: n-hexane) furnished 10-bromo-1-tetrahydropyranyloxydecane (0.30 g, 94percent) as a colourless oil.

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 53463-68-6, 10-Bromodecanol.

Reference:
Article; Kaur, Jasamrit; Kaur, Irvinder; Jindal, Gitanjali; Manhas, Priya; Gupta, Neeru; Singh, Jasvinder; Journal of Chemical Research; vol. 39; 4; (2015); p. 230 – 232;,
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