Tag: M.W=100-200

Electric Literature of 39895-56-2, 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 39895-56-2 as follows.

1-Methyl-4-piperidone (84 muL, 0.73 mmol) was dissolved in methanol (5 mL) and 4-(aminomethyl)benzylalcohol (57MBT52B) (100 mg, 0.73 mmol) was added followed by acetic acid (125 muL). NaBH3CN (92 mg, 1.46 mmol) was added and the mixture was stirred for 3 h. The reaction mixture was evaporated and 2M NaOH (5 mL) was added. Extraction with CH2Cl2 (4*5 mL), drying with Na2SO4 and evaporation gave 152 mg (87%) of N-((4-(hydroxymethyl)phenyl)methyl)-4-amino-1-methylpiperidine (57MBT56D) as a white solid. HPLC-MS (method B) showed MH+=235. UV/MS (%)=100/100.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,39895-56-2, its application will become more common.

Reference:
Patent; ACADIA Pharmaceuticals Inc.; ANDERSSON, Carl-Magnus A.; CROSTON, Glenn; HANSEN, Eva Louise; ULDAM, Allan Kjaersgaard; US2015/259291; (2015); A1;,
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Reference of 5344-90-1 ,Some common heterocyclic compound, 5344-90-1, molecular formula is C7H9NO, 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.

A. 2-Amino-5-bromobenzyl alcohol (1a): A solution of 12.316 g (0.1 mol) of 2-aminobenzyl alcohol in 300 mL of dry ether was treated at about 0° C. with 40.97 g (0.1 mol) of 2,4,4,6-tetrabromocyclohexa-2,5-dienone added in portions with vigorous stirring. Stirring was continued for about 1 hour at about 0° C., then the mixture was extracted twice with dilute HCl. The combined acid extracts were washed with ether and the ether was discarded. The acid solution was made alkaline with NaOH and extracted with fresh ether. The ether extracts were washed with water, brine, dried (Na2 SO4) and concentrated to afford 17.86 g (88percent) of 1a, mp 107-110° C. 1 H NMR (CDCl3): d=7.22-7.17 (m, 2 H); 6.57 (d, 1 H); 4.61 (s, 2 H). (MS (El): m/z=201, 203 (M+, Br isotopes).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,5344-90-1, its application will become more common.

Reference:
Patent; Pfizer Inc.; US5843972; (1998); A;,
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Reference of 2009-83-8, 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 2009-83-8, name is 6-Chlorohexan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

I-a-4-3) (6 g, 43 mmol) p-hydroxybenzoic acid, (7.1 g, 52 mmol) chlorohexanol, (3.44 g, 86 mmol) sodium hydroxide,(0.7g, 4.3mmol) potassium iodide and 50mL water were added to a three-necked flask, heated to reflux, and refluxed for 4 hours,The temperature was lowered, hydrochloric acid was added to the reaction solution, the reaction solution was filtered, and the filter cake was recrystallized twice from ethyl acetate to obtain (6.1 g, 26 mmol) in a yield of 60%

According to the analysis of related databases, 2009-83-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shijiazhuang Cheng Zhiyonghua Display Materials Co., Ltd.; Zhao Lei; Meng Jingsong; Li Ming; Wei Tianyu; Yuan Guoliang; Liang Zhian; (27 pag.)CN110551078; (2019); A;,
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Reference of 4728-12-5 ,Some common heterocyclic compound, 4728-12-5, molecular formula is C7H14O3, 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.

30.1.(2,2-dimethyl-1,3-dioxan-5-yl)methyl 4-methylbenzenesulfonateTo a solution of 1.5 g (10.26 mmol) of (2,2-dimethyl-1,3-dioxan-5-yl)methanol and 1.71 mL of Et3N in 15 mL of DCM, cooled to 0° C., are added 2.15 g (11.3 mmol) of tosyl chloride.The medium is allowed to warm to room temperature, and stirring is continued for 1 hour.The medium is taken up in 100 mL of DCM, washed successively with 0.1N HCl (2*20 mL) and brine (20 mL), dried over Na2SO4, concentrated under reduced pressure and then purified by chromatography on a column of silica gel, eluting with a 99/1 DCM/MeOH mixture.3 g of (2,2-dimethyl-1,3-dioxan-5-yl)methyl 4-methylbenzenesulfonate are obtained in the form of a colourless oil.Yield=97percent1H NMR, CDCl3, 400 MHz, delta (ppm): 7.8 (d, 2H); 7.3 (d, 2H); 4.1 (d, 2H); 3.9 (dd, 2H); 3.6 (dd, 2H); 2.4 (s, 3H); 1.9 (m, 1H); 1.4 (s, 3H); 1.2 (s, 3H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4728-12-5, its application will become more common.

Reference:
Patent; SANOFI; US2011/294788; (2011); A1;,
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Synthetic Route of 1462-03-9, 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. 1462-03-9, name is 1-Methylcyclopentanol. A new synthetic method of this compound is introduced below.

1-methylcyclopentanol (2 mmol), catalytic amounts of the ionic liquid, and 1-2 mL of acetic acid were charged into an oven-dried Schlenk tube under nitrogen. The reaction mass was stirred for 15-20 minutes at r.t. before adding the selected nitrile (1 mmol). The reaction mass was stirred at the indicated temperature for the specified time (see Table 3). The progress of the reaction was monitored by TLC and GC-MS. After completion of reaction, the reaction mass was quenched with distilled water followed by neutralization with dilute NaHCO3 solution. The product was extracted with diethyl ether, dried over anhydrous MgSO4, and the ether layer was evaporated in vacuum. The resulting crude products were chromatographed with hexane-ethyl acetate mixture (80:20) to afford pure colorless solids.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,1462-03-9, its application will become more common.

Reference:
Article; Kalkhambkar, Rajesh G.; Waters, Sarah N.; Laali, Kenneth K.; Tetrahedron Letters; vol. 52; 8; (2011); p. 867 – 871;,
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Related Products of 612-16-8, 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 612-16-8 as follows.

In the glove box, Mn(CO)5Br (0.005mmol), [(E)-2-(2-(1-(2-pyridyl)ethylidene)-indenyl)pyridinium](0.006 mmol),Add 1.0 mL of toluene, stir for two hours, add 2-methylquinoline 4 (2 mmol),2i (1 mmol), after reacting at 135 C for 48 hours, the reaction was stopped, and the solvent was evaporated to dryness.Column chromatography ethyl acetate / petroleum ether (1:10),Trans-disubstituted olefin derivative 3ai. The product was a white solid with a yield of 93%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,612-16-8, its application will become more common.

Reference:
Patent; Qingdao University of Science and Technology; Zhang Chunyan; (19 pag.)CN108250153; (2018); A;,
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Adding a certain compound to certain chemical reactions, such as: 4170-90-5, Mesitylmethanol, 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, name: Mesitylmethanol, blongs to alcohols-buliding-blocks compound. name: Mesitylmethanol

In the glove box, Mn(CO)5Br (0.005mmol),[(E)-2-(2-(1-(2-pyridyl)ethylidene)-indenyl)pyridin](0.006mmol),Add 1.0 mL of toluene, stir for two hours, add 2-methylquinoline 4 (2 mmol)2e (1mmol), after reacting at 135 C for 48 hours, the reaction was stopped, and the solvent was evaporated to dryness.Column chromatography ethyl acetate / petroleum ether (1:10),Trans-disubstituted olefin derivative 3ae. The product was a white solid in 80% yield.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,4170-90-5, Mesitylmethanol, and friends who are interested can also refer to it.

Reference:
Patent; Qingdao University of Science and Technology; Zhang Chunyan; (19 pag.)CN108250153; (2018); A;,
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Synthetic Route of 431-38-9, 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 431-38-9, name is 3-Amino-1,1,1-trifluoropropan-2-ol. This compound has unique chemical properties. The synthetic route is as follows.

A suspension of intermediate Int-21 (1.0 equiv.) and (0487) racemic-3- Amino- l,l,l-trifluoro-propan-2-ol (3.0 equiv.), and triethylamine (5.0 equiv) in 3: 1 dioxane/water (1.3 mL) was heated at 90 C for 12 hours, after which LC-MS analysis indicated that the conversion was complete. The reaction mixture was diluted with water and adjusted to pH 6-7 with 1.0 N aqueous hydrochloric acid solution, leading to the formation of an orange precipitate. The solid was filtered and dried. Purification of the crude solid was achieved by reverse phase HPLC utilizing a gradient of 10 to 40 % acetonitrile in water (modified by 0.1% trifluoroacetic acid) over 20min to afford racemic Compound 1-11 (57.4 mg, 48 % yield) as an off-white solid. 1H NMR: (500 MHz, CD3OD), d (ppm): 9.63 (s, 1 H), 8.61 (s, 1 H), 7.74 (s, 1 H), 7.30 – 7.33 (m, 1 H), 7.15 – 7.20 (m, 1 H), 6.97 – 7.01 (m, 2 H, overlapping shifts), 4.67 (s, 2 H), 4.28 – 4.32 (m, 1 H), 3.98 – 4.02 (m, 4 H, overlapping shifts), 3.86 – 3.91 (m, 1 H). MS ES+ m/z 464.2 [M+H]+

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 431-38-9, 3-Amino-1,1,1-trifluoropropan-2-ol.

Reference:
Patent; CYCLERION THERAPEUTICS, INC.; RENNIE, Glen, Robert; RENHOWE, Paul, Allan; NAKAI, Takashi; MERMERIAN, Ara; CUMBERBATCH, Helen; (99 pag.)WO2019/126354; (2019); 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. 5339-85-5, name is 2-(2-Aminophenyl)ethanol. This compound has unique chemical properties. The synthetic route is as follows. Recommanded Product: 2-(2-Aminophenyl)ethanol

COMPARATIVE EXAMPLE 7 The first run procedures of Example 12 were repeated except that 0.15 g of “NDT-90” was used without K2 CO3 and reaction was continued for 9 hours. The conversion of 2-(o-aminophenyl)ethanol was 12.5% and the yield of indole was 10.8%.

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, 5339-85-5, 2-(2-Aminophenyl)ethanol.

Reference:
Patent; Research Association for Utilization of Light Oil; US4757152; (1988); A;,
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Application of 100058-61-5 , The common heterocyclic compound, 100058-61-5, name is 3-(Benzyloxy)cyclobutanol, molecular formula is C11H14O2, 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.

In a.solution of 2-(5-bromo-3-ethylsulfonyl-2-pyridyl)-3-methyl-6-(trifluoromethyl)imidazo[4,5-c]pyridine(1 g, 2.226 mmol) in methylsulfinylmethane (6 mL) were added dipotassium;carbonate (8.905 mmol,1.231 g) and 3-benzyloxycyclobutanol (6.679 mmol, 1.190 g). The reaction vial was placed inmicrowave and heated at 148 oc for 2 hours. After completion of reaction, reaction mixture was poured into water (60ml ), and the aqueous layer was extracted with ethyl acetate. The combinedorganic layer was washed with aqueous saturated sodium chloride solution (30ml), dried overanhydrous sodium sulfate, and concentrated of under reduced pressure. The residue was purify overreduced pressure.LCMS :- rt 1.13 min ,mass 547 (M+1) 1 H NMR (400 MHz, CHLOROFORM-d) d ppm 1.34- 1.38 (m, 3 H) 2.54- 2.81 (m, 3 H) 2.85- 3.03 (m,2 H) 3.03-3.14 (m, 2 H) 3.77-3.83 (m, 2H) 3.87 (s, 3 H) 4.07-4.16 (m, 1 H) 4.88 (quin, J=6.97 Hz, 1H) 7.79-7.84 (m, 1 H) 8.09-8.12 (m, 1 H) 8.57 (d, J=2.81 Hz, 1 H) 8.95-9.00 (m, 1H).

The synthetic route of 100058-61-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SYNGENTA PARTICIPATIONS AG; RENDLER, Sebastian; EDMUNDS, Andrew; EMERY, Daniel; JUNG, Pierre, Joseph, Marcel; MUEHLEBACH, Michel; RAWAL, Girish; SEN, Indira; SIKERVAR, Vikas; (110 pag.)WO2018/197315; (2018); A1;,
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