Month: August 2021

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. 1072-52-2, name is 2-(Aziridin-1-yl)ethanol, molecular formula is C4H9NO, 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. name: 2-(Aziridin-1-yl)ethanol

(1) Preparation of 1-[2-(2-hydroxyethylamino)ethyl]-4-(4-nitrophenyl)piperazine (compound 75) In 20 ml of chloroform was dissolved 4 g of 1-(4-nitrophenyl)piperazine (compound 66) and 0.52 ml of 1-(2-hydroxyethyl)aziridine, and the solvent was distilled off from the resulting reaction mixture under reduced pressure. To the residue was added 10 mg of Amberlist 15 (trade name; made by Rohm & Haas Co.), and the mixture was then heated with stirring at 100 C. for 3 hour. Afterward, the temperature of the reaction mixture was returned to room temperature. To the reaction mixture was added 20 ml of chloroform, and insoluble matters were then removed therefrom by filtration. The filtrate was concentrated, and the resulting residue (concentrate) was purified through a silica gel column chromatograph (chloroform/methanol=100/1 to 25/1 in terms of volume ratio), thereby preparing 1 g of 1-[2-(2-hydroxyethylamino)ethyl]-4-(4-nitrophenyl)piperazine (compound 75).

With the rapid development of chemical substances, we look forward to future research findings about 1072-52-2.

Reference:
Patent; Mitsui Toatsu Chemicals, Incorporated; US5008267; (1991); A;,
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Application of 25574-11-2, 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.25574-11-2, name is 3-(4-Bromophenyl)propan-1-ol, molecular formula is C9H11BrO, molecular weight is 215.087, as common compound, the synthetic route is as follows.

General procedure: An evacuated and argon purged 250 mLthree-necked round-bottom flask equipped with a Teflon-coated magnetic stirringbar, argon inlet, reflux condenser and gas bubbler was charged with30.0 mmol (1.0 eq) 4-bromoaryl derivative. It was dissolved in60 mL degassed EtOH:H2O = 7:3 (v/v) under argon and 3.90 g(60.0 mmol, 2.0 eq) NaN3, 297 mg (1.50 mmol, 5.0 mol %)sodiumascorbate, 571 mg (3.00 mmol, 10 mol%) as well as 485 muL (397 mg,4.50 mmol, 15 mol%) N,N?-dimethylethylenediamine(DMEDA) were added, respectively. The bluish suspension wasadditionally degassed for three times applying vacuum to the suspension untilthe solvent started to boil, which was immediately afterwards purged withargon. It was heated under reflux in an oil bath at 100 C for 2 huntil reaction control via GC-MSshowed quantitative conversion of the starting material. Subsequently, the bluishsuspension was cooled to room temperature and the solvent was removed on arotary evaporator. The residual, brownish solid was diluted with 300 mLEtOAc and the organic phase was washed with 1 M HCl (2 x 150 mL).Afterwards the product was re-extracted from the brownish, aqueous phase withEtOAc (1 x 50 mL), the combined brownish, organic phases were washed withhalf-saturated NaHCO3 (2 x 150 mL) and again re-extracted withEtOAc (1 x 50 mL). The combined yellowish, organic phases were dried overMgSO4, filtered, and concentrated on a rotary evaporator. Finally, the brownish, viscous liquid was purified via flash column chromatography(250 g SiO2, column: 22.0 x 6.0 cm) and the resultingyellowish liquid dried under high vacuum.

The chemical industry reduces the impact on the environment during synthesis 25574-11-2, I believe this compound will play a more active role in future production and life.

Reference:
Article; Leypold, Mario; Wallace, Paal W.; Kljajic, Marko; Schittmayer, Matthias; Pletz, Jakob; Illaszewicz-Trattner, Carina; Guebitz, Georg M.; Birner-Gruenberger, Ruth; Breinbauer, Rolf; Tetrahedron Letters; vol. 56; 41; (2015); p. 5619 – 5622;,
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Application of 163119-16-2, 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. 163119-16-2, name is 2,6-Di-tert-butyl-4-methylcyclohexanol, molecular formula is C15H30O, 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.

To a mixture of 186 g of Compound (I-7) and 272 g of the foregoing Intermediate (I-6) suspended in 1.4 liter of ethyl acetate, 161 g of potassium acetate and 387 ml of anhydrous acetic acid were added in this order and stirred at 45 C. for 3 hours on a steam bath to react them. Thereafter, the reaction mixture was cooled on an ice bath and then 1 liter of water was added. Following stirring for 1 hour while cooling on an ice bath, precipitated crystals were collected by filtration. The crystals were washed with water. Crystals thus obtained were suspended in 1.5 liters of methanol and then 400 ml of a 25% aqueous ammonia was added. The resulting mixture was stirred at 40 C. for 3 hours on a hot water bath and then cooled on an ice bath and subjected to neutralization with dilute hydrochloric acid. Precipitated crystals were collected by filtration. The crystals were washed with water and dried. As a result, 291 g (yield 66%) of the objective Intermediate (I-8) was obtained, as a white crystal.

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 163119-16-2, 2,6-Di-tert-butyl-4-methylcyclohexanol.

Reference:
Patent; Fuji Photo Film Co., Ltd.; US6649771; (2003); B2;,
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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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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;,
Alcohol – Wikipedia,
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Related Products of 94022-96-5, Adding some certain compound to certain chemical reactions, such as: 94022-96-5, name is 2-(Trifluoromethyl)phenethyl alcohol,molecular formula is C9H9F3O, 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 94022-96-5.

General procedure: A mixture of the substituted phenylethyl alcohol (10 mmol), Chloromethyl methyl ether (15mmol) and N,N-diisopropylethylamine (20 mmol) in dry dichloromethane (25 mL)was stirred under nitrogen atmosphere for 2.5 h at rt. The reaction mixture wasthen washed with water (2×50 mL), dried (NaSO4) and the solvent wasremoved in vacuo. The crude MOM acetal was dissolved in dried CH3CN (25mL) and added to cooled (0 oC) solution of Trimethylsilyltrifluoromethanesulfonate (TMSOTf) (10 mmol). The reaction was carried outunder nitrogen atmosphere for 3 h. Then the mixture was quenched by theaddition of l M NaHCO3 (20 mL ). The orgnic phase was washed withbrine (2×50 mL), dried (NaSO4) and evaporated under reducedpressure. Purification by FC afforded relevant substituted isochromans.

According to the analysis of related databases, 94022-96-5, the application of this compound in the production field has become more and more popular.

Reference:
Article; Zhou, Mei-Yan; Kong, Shan-Shan; Zhang, Ling-Qiong; Zhao, Ming; Duan, Jin-Ao; Ou-Yang, Zhen; Wang, Min; Tetrahedron Letters; vol. 54; 30; (2013); p. 3962 – 3964;,
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Application of 629-41-4, 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. 629-41-4, name is 1,8-Octanediol, molecular formula is C8H18O2, 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.

The compound 2-1-1 (octanediol) (1.01 g, 6.91 mmol) was dissolved in 20 ml of toluene, and 40% HBr (aq) (1.12 ml, 7.81 mmol) was added to the reaction system at room temperature, bath reflux.72h after TLC monitoring, there is still the remaining raw materials, add 40% HBr (aq) (0.5ml, 3.49mmol), continue to return 24h.The system was cooled to room temperature, diluted with ether, saturated sodium bicarbonate solution, saturated sodium chloride solution, washed once, sodium sulfate dried about half an hour after the filter, steamed ether.The residue was purified by column chromatography on silica gel, eluting with petroleum ether: ethyl acetate = 6: 1 to give an oily product, 1.21 g, in 84.3% yield.

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 629-41-4, 1,8-Octanediol.

Reference:
Patent; PEKING UNIVERSITY; YE, XINSHAN; HOU, JINGFEI; (25 pag.)CN103373955; (2016); B;,
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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. 56456-51-0, name is 2-Chloro-4-(trifluoromethyl)benzyl alcohol, the common compound, a new synthetic route is introduced below. SDS of cas: 56456-51-0

To a solution of 2-chloro-4-trifluoromethylbenzyl alcohol (38.8 g) and pyridine (3.0 ml) in diethyl ether (320 ml)- tetrahydrofuran (80 ml) was added thionyl chloride (32.8 g) , and the mixture was stirred at room temperature for 15 hr. The reaction solution was concentrated, water was poured’ into the residue and the mixture was extracted with ethyl acetate. The o ethyl acetate layer was washed with IN hydrochloric acid, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, dried (MgSO4), and concentrated. The residue was subjected to silica gel column chromatography, and eluted with ethyl acetate-hexane (1:25 – 1:12, v/v) to give 2-chloro- 4-trifluoromethylbenzyl chloride (38.9 g, yield: 92%) as a colorless oil.1H-NMR (300 MHz, CDCl3) delta:4.72 (2 H,, s) , 7.51 – 7.57 (1 H, m) , 7.60 – 7.70 (2 H, m) .

The synthetic route of 56456-51-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; WO2007/18314; (2007); A2;,
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Adding a certain compound to certain chemical reactions, such as: 929-06-6, 2-(2-Aminoethoxy)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, 929-06-6, blongs to alcohols-buliding-blocks compound. Quality Control of 2-(2-Aminoethoxy)ethanol

Step 1 2-(2-N-Boc-aminoethoxy)ethanol To a solution of 2-(2-aminoethoxy)ethanol (5.3 g, 50 mmol) and diisopropylethylamine (13 ml, 75 mmol) in DCM (10 ml) at 0 C. was added dropwise a is solution of di-tert-butyl dicarbonate (12 g, 55 mmol) in DCM (20 ml). The reaction was agitated for 4 hours, extracted with DCM and purified by flash chromatography (EtOAc/PE) (75/25) to give the title compound (5.9 g, 60%). 1H NMR (CDCl3) delta 3.65 (dd, J=8.6, 3.8 Hz 2H), 3.47 (m, 5H), 2.23 (dd, J=8.6, 3.8 Hz 2H), 1.35 (s, 9H); 13C NMR (CDCl3) delta 56.1, 79.1, 72.1, 70.1, 61.3, 40.3, 28.2.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,929-06-6, its application will become more common.

Reference:
Patent; Gustavsson, Anna-Lena; Jendeberg, Lena; Roussel, Patrick; Slater, Martin; Thor, Markus; US2003/73862; (2003); A1;,
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Electric Literature of 534-03-2, 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.534-03-2, name is 2-Aminopropane-1,3-diol, molecular formula is C3H9NO2, molecular weight is 91.1091, as common compound, the synthetic route is as follows.

Intermediate 131: 2-(l,3-Dihvdroxypropan-2-yl)isoindoline-l,3-dione (0848) To a stirring solution of 2-aminopropane-l,3-diol (327.2 mg, 3.59 mmol, commercially available from, for example, Sigma-Aldrich) in DMF (15 ml.) was added phthalic anhydride (533.6 mg, 3.60 mmol) portionwise. The resulting colourless solution was stirred at 90 C under nitrogen for 5 h, after which the reaction mixture was cooled to rt and the volatiles evaporated in vacuo. This was partitioned between ethyl acetate (25 ml.) and water (25 ml.) and the layers separated. The aqueous phase was extracted with further ethyl acetate (4 x 25 ml.) and the organic layers combined and filtered through a cartridge fitted with a hydrophobic frit. The filtrate was evaporated in vacuo. This was redissolved in ethyl acetate (approx. 4 ml.) and 3: 1 ethyl acetate :ethanol (approx. 4 ml.) and directly applied to the top of a 25 g SNAP cartridge and purified by flash column chromatography. The column was eluted with a gradient of 0% – 40% (3: 1 ethyl acetate:ethanol) in cyclohexane. The appropriate fractions were combined and evaporated in vacuo to give 2-(l,3-dihydroxypropan-2- yl)isoindoline-l,3-dione (380.0 mg, 1.72 mmol, 48 % yield) as a white solid. (0849) LCMS (2 min High pH): Rt = 0.55 min, [MH]+ = 222.3.

The chemical industry reduces the impact on the environment during synthesis 534-03-2, I believe this compound will play a more active role in future production and life.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; ATKINSON, Stephen John; DEMONT, Emmanuel Hubert; HARRISON, Lee Andrew; LEVERNIER, Etienne; PRESTON, Alexander G; SEAL, Jonathan Thomas; WALL, Ian David; WATSON, Robert J; WOOLVEN, James Michael; (225 pag.)WO2017/174621; (2017); A1;,
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