Tag: M.W=100-200

Electric Literature of 1805-32-9, Adding some certain compound to certain chemical reactions, such as: 1805-32-9, name is 3,4-Dichlorobenzyl alcohol,molecular formula is C7H6Cl2O, 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 1805-32-9.

Under nitrogen, 4-aminobenzenesulfonamide (172 mg, 1 mmol), [Cp * IrCl2] 2 (8 mg, 0.01 mmol,1 mol%), cesium carbonate (65 mg, 0.2 mmol), 3,4-dichlorobenzyl alcohol (212 mg, 1.2 mmol)The alcohol (1.0 mL) was added sequentially to a 25 mL Schlenk reaction flask. The mixture was reacted at 120 C for 12 hoursAfter cooling to room temperature, the solvent was removed under vacuum. And then purified by column chromatography (developing solvent: ethyl acetate / n-hexane)The pure title compound was obtained in a yield of 92%

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. 1805-32-9, 3,4-Dichlorobenzyl alcohol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NANJING UNIVERSITY OF SCIENCE AND TECHNOLOGY; LI, FENG; LU, LEI; MA, JUAN; (16 pag.)CN106146358; (2016); A;,
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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 623-69-8, name is 1,3-Dimethoxypropan-2-ol. This compound has unique chemical properties. The synthetic route is as follows. HPLC of Formula: C5H12O3

To a solution of 3-bromophenol (6g, 34.7mmol) and 1,3-dimethoxypropan-2-ol (5.OOg,41.6mmol) in THE (l5OmL) was added triphenylphosphine (13.64g, 52.Ommol) and the reaction mixture cooled to 0C followed by dropwise addition of DIAD (6.74mL, 34.7mmol). The reaction was allowed to warm to room temperature, then stirred for 12h. The reaction mixture was concentratedvacua. The obtained residue was dissolved in EtOAc (SOmL), washed with water (SOmL) and brine(SOmL), dried over Na24, concentrated in vacua and subjected to silica column chromatography(SOg column), eluting with 20% EtOAc in petroleum ether. The relevant fractions were combined andconcentrated in vacua affording the title compound (4.Og, 42%) as a yellow liquid: MS ES+ve m/z275, 277 (M–H).

With the rapid development of chemical substances, we look forward to future research findings about 623-69-8.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ANDERSON, Niall Andrew; CAMPBELL-CRAWFORD, Matthew Howard James; HANCOCK, Ashley Paul; LEMMA, Seble; PRITCHARD, John Martin; PROCOPIOU, Panayiotis Alexandrou; REDMOND, Joanna Mary; SOLLIS, Steven Leslie; (77 pag.)WO2017/162572; (2017); A1;,
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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.79418-41-0, name is 3-Amino-7-hydroxy-2H-chromen-2-one, molecular formula is C9H7NO3, molecular weight is 177.1568, as common compound, the synthetic route is as follows.Recommanded Product: 79418-41-0

A portion of 7-diethylaminocoumarin-3-aldehyde (247 mg, 1 mmol) and 3-amino-7-hydroxycoumarin (195 mg, 1.1 mmol) were combined in hot absolute ethanol (20 mL) to yield a scarlet precipitate for a moment. The solution was stirred under reflux conditions for 6 h, and the precipitate was filtrated, washed with hot absolute ethanol three times, then recrystallized with DMF/H2O (v/v, 1/3) to get scarlet crystal L (347 mg, 0.86 mmol) in 86% yield. IR (KBr, cm-1): 2966, 2927, 1718, 1620, 1349, 1506, 1456, 1420, 845, 811, 770, 729, 693. 1H NMR (DMSO-d6, 400 MHz, delta): 10.54(s, 1H, OH), 9.04(s, 1H, NCH), 8.56(s, 1H, ArH), 7.81(s, 1H, ArH), 7.70(d, 1H, J = 12 Hz, ArH), 7.58(d, 1H, J = 8 Hz, ArH), 6.81 (t, 1H, J = 8 Hz, ArH), 6.77 (s, 1H, ArH), 6.61(s, 1H, ArH), 3.49(q, 4H, J = 8 Hz, CH2CH3), 1.16(t, 6H, J = 8 Hz, CH2CH3). Anal. Calcd for C23H20N2O5: C 68.31%, H 4.98%, N 6.93%, Found: C 68.55%, H 5.04%, N 6.66%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,79418-41-0, 3-Amino-7-hydroxy-2H-chromen-2-one, and friends who are interested can also refer to it.

Reference:
Article; Wang, Lingyun; Ye, Decheng; Cao, Derong; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 90; (2012); p. 40 – 44;,
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Adding a certain compound to certain chemical reactions, such as: 26021-57-8, 3,4-Dihydro-2H-benzo[b][1,4]oxazin-6-ol, 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, 26021-57-8, blongs to alcohols-buliding-blocks compound. COA of Formula: C8H9NO2

General procedure: To a mixture of 9 (100mg, 0.74mmol) (the general procedure for the synthesis of intermediate 9 was presented in supporting information), 3-chlorobenzaldehyde (104mg, 0.74mmol) and ethyl 2-cyanoacetate (83muL, 0.78mmol) in anhydrous EtOH (5mL) was added piperdine (136muL, 1.48mmol). The reaction mixture was stirred for 16hat 80C under N2 atmosphere. The resulting reaction mixture was evaporated to dryness under reduced pressure. The residue was purified by flash column chromatography eluting with CH2Cl2/MeOH (200:1-100:1, v/v) to afford the title compound (9a) as a slight yellow solid (210mg, 77% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,26021-57-8, its application will become more common.

Reference:
Article; Zhang, Huijun; Fang, Xiong; Meng, Qian; Mao, Yujia; Xu, Yan; Fan, Tingting; An, Jing; Huang, Ziwei; European Journal of Medicinal Chemistry; vol. 157; (2018); p. 380 – 396;,
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Electric Literature of 3319-15-1 ,Some common heterocyclic compound, 3319-15-1, molecular formula is C9H12O2, 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.

General procedure: To a mixture of 1,3-dicarbonyl compound (2 mmol),alcohol or styrene derivatives (1 mmol), and 0.6 gSBNPSA, was added 2 cm3 nitromethane as solvent. Themixture was stirred under reflux conditions and the reactionwas followed by TLC. After completion, the mixture wasfiltered, and the remaining was washed with warm ethanolto separate catalyst and nitromethane was removed underreduced pressure. Then, the crude products were recrystallizedfrom mixture of dichloromethane and n-hexane.All the synthesized products were known and characterized by comparison of their spectral and physical data withthose reported in literature.

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. 3319-15-1, 1-(4-Methoxyphenyl)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Karimzadeh, Morteza; Saberi Asl, Hamed; Hashemi, Hajar; Saberi, Dariush; Niknam, Khodabakhsh; Monatshefte fur Chemie; vol. 149; 12; (2018); p. 2237 – 2244;,
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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. 1777-82-8, name is (2,4-Dichlorophenyl)methanol, the common compound, a new synthetic route is introduced below. HPLC of Formula: C7H6Cl2O

General procedure: In a general process, the photocatalytic activity of nanostructureswas investigated by oxidation of aromatic alcohol. In typically,0.1 mmol of alcohol was added to 1.5 ml of solvent in Pyrex glass celland stirred for 5 min. Then, 10 mg of photocatalyst was dispersed insolution and magnetically stirred in the dark for 15 min to reach anequilibrium between adsorption-desorption. Photocatalytic reactionswere performed by irradiation with an LED lamp (5 W). To control thetemperature during the oxidation reaction, the water circulation wasapplied to cooling of the reaction mixture. During the photocatalyticprocess, the reactor was exposed to air to ensure that enough oxygen isprovided for the reaction. The progress of the reaction was monitoredusing the TLC by periodic sampling. After completion of the reaction,the catalyst was separated from the suspension by centrifuging(3500 rpm) and washed with solvent to separate all of the residualmaterials.

The synthetic route of 1777-82-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Safaei, Elham; Mohebbi, Sajjad; Journal of Photochemistry and Photobiology A: Chemistry; vol. 371; (2019); p. 173 – 181;,
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Application of 6338-55-2 ,Some common heterocyclic compound, 6338-55-2, molecular formula is C6H15NO3, 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.

See FIG. 22 for the synthesis of DBCO-PEG-OH (compound [IV]). To a solution of 2- (2- (2-aminoethoxy) ethoxy) ethan-1-ol (compound [I], 0.267 g, 1.789 mmol) in 2 ml anhydrous DCM at RT was added DBCO- (Compound [II], 0.24 g, 0.596 mmol) in DMF (5 mL) was slowly added.After the addition is complete,The reaction solution was stirred for 2 hours at RT. HPLC showed complete disappearance of the succinimide. The reaction was maintained in the dark at -20 C in the freezer.The next morning,The reaction solution was warmed below RT and diluted with 3 ml DCM.Silica gel (5 g) was added and the slurry was evaporated to dryness on a rotary evaporator.Loading the remaining powder onto the ISCO loading cartridge,Purification by column chromatography (12 g silica gel column, 5-20% methanol / DCM)0.2 g of DBCO-PEG-OH (compound [IV]) was obtained. Yield: 77%

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,6338-55-2, its application will become more common.

Reference:
Patent; Roseuwel Bio Tekeu Nol Ro Jiseu In Kopo Lei Tideu; Me Ri-meon-bae-ri-el; Ga I-jeo-tim; Mol Ra-pol-deo-beul-yu; Ra I-deu-a-us-de-ril; (101 pag.)KR2019/34320; (2019); A;,
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Application of 6351-10-6, 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. 6351-10-6, name is 2,3-Dihydro-1H-inden-1-ol. A new synthetic method of this compound is introduced below.

General procedure: A mixture of alcohol 1a (100 mg, 0.54 mmol), alkene 2a (43 mg, 0.54 mmol), Ca(OTf)2 (18.3 mg, 0.05 mmol),Bu4NPF6 (21 mg, 0.05 mmol) was heated under solvent free condition at 70C for 1.5 h until complete consumption of the starting material as monitored by TLC. After the completion of the reaction the mixture was purified by flash column chromatography (petroleum ether) to afford the desired product 3a.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,6351-10-6, its application will become more common.

Reference:
Article; Yaragorla, Srinivasarao; Pareek, Abhishek; Dada, Ravikrishna; Almansour, Abdulrahman I.; Arumugam, Natarajan; Tetrahedron Letters; vol. 57; 52; (2016); p. 5841 – 5845;,
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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.623-04-1, name is (4-Aminophenyl)methanol, molecular formula is C7H9NO, molecular weight is 123.1525, as common compound, the synthetic route is as follows.Quality Control of (4-Aminophenyl)methanol

The specific process is: 4-aminobenzyl alcohol (1.48g, 12mmol) with 4N sulfuric acid (15mL) is dissolved, and cooled to 0 C. then sodium nitrite (1.66 g, 24 mmol) was dissolved in water (10 mL) and dissolved, and then added dropwise. after controlling the temperature at 0 C for 30 min. sodium azide (2.34 g, 36 mmol) was dissolved in water (10 mL), and added dropwise to the above reaction solution, and slowly warmed to room temperature for 1 h. After completion of the reaction, the mixture was extracted with ethyl acetate. The organic phase was combined, and the organic phase was washed with a saturated sodium chloride solution, and the organic phase was dried over anhydrous sodium sulfate. Purified with petroleum ether / 0-10% ethyl acetate)The product was obtained as a yellowish solid, 4-azidobenzyl alcohol, yield 90%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,623-04-1, (4-Aminophenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; Hezhou College; Zhu Dongjian; Ren Aishan; Cai Wen; Duan Zhenhua; (20 pag.)CN109134344; (2019); A;,
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Electric Literature of 104-38-1, 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.104-38-1, name is 1,4-Bis(2-hydroxyethoxy)benzene, molecular formula is C10H14O4, molecular weight is 198.2158, as common compound, the synthetic route is as follows.

Example 120 2-[4-(2-{[3-(1-Piperazinyl)-2-pyrazinyl]oxy}ethoxy)phenoxy]ethanol, Maleate The title product was prepared from 1,4-bis(2-hydroxyethoxy)benzene. Yield of free base of the title compound 51%. The maleate salt was prepared: mp 127-129 C. MS m/z 361 (M+H). Anal. (C18H24N4O4.C4H4O4) C, H, N.

The chemical industry reduces the impact on the environment during synthesis 104-38-1, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Biovitrum AB; US6465467; (2002); B1;,
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