Month: August 2021

Related Products of 461432-23-5, These common heterocyclic compound, 461432-23-5, name is 4-Bromo-1-chloro-2-(4-ethoxybenzyl)benzene, 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.

Add compound 3a (180g, 0.55mol), tetrahydrofuran (360ml), toluene (720ml) to a 5L three-necked flask, stir until dissolved, nitrogen protection, dry ice-acetone bath to -80 ~ -70 C, add n-butyl Lithium-based solution (287 ml, 0.715 mol, 1.3 eq), the dropwise addition process control temperature was -80 to -70 C, and the reaction was stirred at -80 to -70 C for 0.5 h after the completion of the dropwise addition. A solution of Compound 2a (400 g, 0.86 mol) in toluene (360 ml) was added dropwise, and the dropwise addition process was carried out at -80 to -70 C, and the reaction was stirred at -80 to -70 C for 1 hour after the dropwise addition.A solution of trifluoroacetic acid (126 g, 1.10 mol) dissolved in water (600 mL) was added dropwise to the reaction solution, and the temperature was controlled to be less than -20 C. After the completion of the dropwise addition, the temperature was naturally raised to 10 to 20 C, and the reaction was carried out for 2 to 3 hours.After completion of the reaction, water (180 ml) and ethyl acetate (180 ml) were added, and the mixture was stirred for 30 min. Wash with saturated aqueous sodium hydrogencarbonate (720 ml) and water (720 ml), dry over anhydrous sodium sulfate (400 g)Concentrated under reduced pressure at 42 C to dryness to give compound 4a (230 g).The yield was 98.4%.

The synthetic route of 461432-23-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Haosen Pharmaceutical Group Co., Ltd.; Yu Jun; Yu Haizhou; Wang Jinjia; Cao Yin; Du Zuyin; (8 pag.)CN108610316; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, A new synthetic method of this compound is introduced below., COA of Formula: C6H4ClN3

4-Nitro-5-chloro-1H-benzotriazole [22] 5-Chloro-1H-benzotriazole (3.08g, 20mmol) was dissolved in conc. sulphuric acid (40ml) and cooled to 0C on an ice bath. Nitric acid (40ml, excess) was added drop wise to the cooled solution over a period of 20 minutes. Stirring was continued for 1 hour at 0C and then at 60C for an additional 1 hour, by which time TLC (A) indicated the conversion of starting material. The solution was cooled to room temperature and poured over ice to precipitate a white solid. The solid was collected by filtration and washed with copious amounts of water until neutral to afford [22] in 83% yield. Rf(A) 0.49 deltaH(400MHz; DMSO-d6) 7.75 (1H, d, J8.8, BT) 8.38 (1H, br s, BT); m/z (EI-HR) 197.99383 [(M) calc. for C6H3N4O235Cl 197.99445] and 199.99345 [(M) calc. for C6H3N4O2 37Cl 199.99150].

The synthetic route of 94-97-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; University of Strathclyde; EP1272827; (2008); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. 367-22-6, name is 4-Chloro-3-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H5ClFN

Compound 102[00318] 4-Chloro-3-fluoroaniline; (250.3g, 1.719mol) was added to a 5L four-neck round bottom flask equipped with overhead stirrer, reflux condenser, heating mantle, temperature controller, an internal temperature probe and an argon inlet. r°-Heptane (2000ml) and di-t- butyl-dicarbonate (450.3g, 2.064mol) were charged to the flask. The mixture was stirred under argon at room temperature for 15min allowing dissolution of the majority of the solids. The mixture was heated to reflux for 4h under argon (care: generation of CO2 g). Analysis of the reaction mixture by HPLC method Test 20 (THFrMeCN 1 :1) indicated complete conversion of starting material (Rt 4.57min) to one product (Rt 6.17min). [00319] The reaction was allowed to cool to 50-550C and transferred in two portions to a 3 L one-neck RBF. A total of 1500ml of distillate was removed by concentration in vacuo at 450C to give a peach colored solution with white crystals. The slurry was allowed to cool to room temperature, whilst stirring, for 1.5h. The flask was stored at 40C for 15h after which time the crystals were filtered under vacuum and washed with cold «-heptane (400ml). [00320] After drying at 350C under vacuum for 7h, very fine, white crystals of Compound 102 (393.1g, 93% yield) were obtained. Compound 102: C?Hi3ClFNO2 245.68gmol”. HPLC analysis (Test 20, MeCN): R1 6.16min; 99% purity (at) 254nm. m.p.: 103-1040C. 1H NMR OH (400 MHz, CDCl3): 1.51 (9H, s, 3 x CH3), 6.56 (IH, br-s, N-H), 6.94, 7.25, 7.35 (3 x 1Eta, 3 x m, 3 x Ar-H).

According to the analysis of related databases, 367-22-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; IDENIX PHARMACEUTICALS, INC.; WO2008/42240; (2008); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 41965-95-1, The chemical industry reduces the impact on the environment during synthesis 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride, I believe this compound will play a more active role in future production and life.

Methyl 2-ch]oro^-[(3-chloro^-methoxybenzyi)amino]-6-cyanoquinoime-3- carboxylate, 14 [00171] To a heterogenous mixture of quinoline 13 (3.56 mmol) and 3-chloro-4-methoxy benzylamine-HCl (3.92 mmol) in NMP (15 mL) was added ‘Pr2NEt (8.90 mmol). The reaction mixture was heated to 80 C for 3 h. Subsequently, cooled the reaction mixture to ambient temperature and added 1M aqueous HC1 and EtOAc. The resulting layers were separated and the organic layer washed with water (3x) followed by brine (lx). The combined organic layers were dried over Na2S04, filtered, and concentrated in vacuo. The residue was dissolved in a minimum amount of hot EtOAc and allowed to cool to ambient temperature. Hexanes was then added to the solution and the intermediate 14 (80% yield) precipitated out and was collected by vacuum filtration. lU NMR (300 MHz, CDCI3) delta 8.20 (s, I I I ). 7.95 (d, i Pi. ./ 8.4 Hz), 7.82 (d, 1 1 1. 7 5 Hz), 7.38 (s, 1 H), 7.27-7.22 (m, 1H), 6.98 (d, 1 H, J=8.4 Hz), 6.26 is, 1H), 4.54 id, 2H J=4.8 Hz), 3.95 (s, 3H), 3.93 (s, 3H).

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, 3-Chloro-4-methoxybenzylamine Hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; LANDRY, Donald, W.; DENG, Shixian; FIORITO, Jole; ARANCIO, Ottavio; WASMUTH, Andrew; WO2015/9930; (2015); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 104-77-8, 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. 104-77-8, name is 3-Chloro-N,N-diethylpropan-1-amine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 46 3-[1-(3-Diethylaminopropyl)-4-piperidyl]-1,2-benzisoxazole difumarate A suspension of 4.0 g of 3-(4-piperidyl)-1,2-benzisoxazole, 3.2 g of 3-diethylaminopropyl chloride, 3.0 g of potassium iodide and 5.0 g of sodium bicarbonate in 100 ml of butanol was heated under reflux for 2 hrs, cooled to room temperature and filtered. The filitrate was washed with water and extracted with ether (3 times). The ether extracts were dried over anhydrous sodium sulfate, filtered and evaporated to give an oil. The oil was dissolved in 10 ml of acetonitrile and 4.2 g of fumaric acid was added. The mixture was stirred for 2 hrs, filtered and the filter cake was recrystallized three times from ethanol-ether to give 2.8 g (26%) of product, mp 174-176. ANALYSIS: Calculated for C19 H29 N3 O2C4 H4 O4: 59.22%C; 6.81%H; 7.67%N; Found: 59.26%C; 7.01%H; 7.33%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, 3-Chloro-N,N-diethylpropan-1-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hoechst-Roussel Pharmaceuticals; US4355037; (1982); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 7006-52-2, name is N-Methyl-3-chloroaniline, 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. Formula: C7H8ClN

General procedure: To a solution of 13 (500 mg, 1.86 mmol) in DMF (5.0 mL) were added N-methylaniline (241 muL, 2.23 mmol), 1-hydroxybenzotriazole (251 mg, 1.86 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (534 mg, 2.79 mmol) at room temperature. The reaction mixture was stirred at room temperature for 12 h. Water was then added, and the mixture was extracted with a mixture of toluene and EtOAc (1:1). The organic layer was washed with H2O and brine, and dried over anhydrous sodium sulfate. After filtration, the solvent was removed in vacuo, and the residue was purified by silica gel column chromatography using hexane/EtOAc (1:1, v/v) as eluent. The solvent was removed in vacuo, and the resulting solid was recrystallized from iPrOH to give 14 (547 mg, 82percent) as a white solid

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

Reference:
Article; Fukaya, Takayuki; Kodo, Toru; Ishiyama, Takeo; Kakuyama, Hiroyoshi; Nishikawa, Hiroyuki; Baba, Satoko; Masumoto, Shuji; Bioorganic and Medicinal Chemistry; vol. 20; 18; (2012); p. 5568 – 5582;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 445-13-6, 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. 445-13-6, name is 3-Chloro-4-(trifluoromethyl)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of 6 (0.13 mmol, 1 eq) in THF (0.5 mL, 0.26M) in a 1-dram vial at room temperature aniline/heterocyclic amine (0.13 mmol, 1 eq) was added in one portion. The vial was sealed and the mixture heated to reflux for 16 hours to yield crude 7. For compounds 8, after cooling to room temperature, N,N-Diisopropylethylamine (0.143 mmol, 1.1 eq) and isobutyl chloroformate (0.143 mmol, 1.1 eq) were added and the reaction was stirred for 30 minutes at room temperature. For primary carboxamide congeners, ammonium hydroxide (1mL) was added and the reaction was stirred for an additional hour at room temperature. For substituted amide analogs, desired amine (0.26, 2 eq) was added instead of ammonium hydroxide and stirring was continued for an additional 2 hours. The reaction was then diluted with ether (1mL), the layers were separated and the aqueous layer was extracted with ether (3x2mL). The organic layers were passed through a phase separator and concentrated in vacuo, and then crude product was purified using preparative HPLC (30x50mm column, MeCN/0.1% TFA: Water, 4 min gradient) to yield desired compounds 8.

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, 3-Chloro-4-(trifluoromethyl)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Fulton, Mark Gallant; Loch, Matthew Thomas; Cuoco, Caroline Anne; Rodriguez, Alice Lambert; Days, Emily; Vinson, Paige Newton; Kozek, Krystian Andrezej; Weaver, Charles David; Blobaum, Anna Louise; Conn, Peter Jeffrey; Niswender, Colleen Marie; Lindsley, Craig William; Letters in drug design and discovery; vol. 16; 12; (2019); p. 1387 – 1394;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1127-85-1, These common heterocyclic compound, 1127-85-1, name is 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline, 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 title compound in this step was prepared according to the method described in step 4 of Example 4, ie, 2,4_dichloro_5,6,7,8-tetrahydroquinazoline (3.21 g, 15.8 lmmo 1) and sodium hydroxide solution (100mL, 1mol/L) and tetrahydrofuran (12mL)Reaction at 60C for 12h. The obtained crude product was separated and purified by silica gel column chromatography (petroleum ether/ethyl acetate (nu/nu) = 4/1) to obtain the standardThe title compound (white solid, 2.61g, 91%).

Statistics shows that 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline is playing an increasingly important role. we look forward to future research findings about 1127-85-1.

Reference:
Patent; GUANGDONG HEC PHARMACEUTICAL; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; JIN CHUANFEI; Jin Chuanfei; LAO JINHUA; Lao Jinhua; ZHANG YINGJUN; Zhang Yingjun; (35 pag.)CN108299437; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 623-12-1,Some common heterocyclic compound, 623-12-1, name is 1-Chloro-4-methoxybenzene, molecular formula is C7H7ClO, 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.

EXAMPLE 6 The general procedure from Example 1A was followed using 4-chloroanisole (171 mg, 1.2 mmol) and piperidine (100 mul, 1.0 mmol) with Pd2(dba)3 (20 mg, 0.0218 mmol) and (Me3C)2PH(O) (14.5 mg, 0.0878 mmol) and NaOtBu (144 mg, 1.5 mmol) in 4.0 mL of toluene. After 12 h, the reaction mixture was chromatographed with 5% ethyl acetate/hexane to give 128 mg (67% yield) of N-(4-methoxyphenyl)piperidine. It was >95% pure by 1H NMR and GC/MS. 1H NMR (500 MHz, CDCl3): delta 6.81 (d, J=9.11 Hz, 2H), 6.72 (d, J=9.11 Hz, 2H), 3.65 (s, 3H), 2.92 (t, J=5.46 Hz, 4H), 1.60 (m, 4H), 1.46 (m, 2H) ppm. 13C NMR (125 MHz, CDCl3): delta 153.5, 146.8, 118.6, 114.3, 55.4, 52.2, 26.1, 24.1 ppm.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Chloro-4-methoxybenzene, its application will become more common.

Reference:
Patent; Li, George Y.; US2002/137974; (2002); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 93-50-5, name is 4-Chloro-2-methoxyaniline, belongs to chlorides-buliding-blocks compound, 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 93-50-5, category: chlorides-buliding-blocks

General procedure: Aniline (0.94 g,0.010 mol) was added dropwise, with stirring, to syrupy phosphoricacid (15 mL) at 0C. Finely ground sodiumnitrite (0.83 g,0.012 mol) was added with stirring over 15 min. This solutionwas allowed to stand at 0C for ca. 1 h after which time urea(ca. 100 mg) was added to destroy unreacted nitrite. After a further30min at 0C, a solution of freshly distilledmercaptoaceticacid (0.92 g, 0.010 mol) in water (250 mL) at 0C was addedswiftlywithvigorous stirring,maintainingapHof ca. 4. After ca.1 h of stirring at 0C, a dense pale buff precipitate had formed.The suspension was then filtered, washed with distilled waterand dried in a vacuum desiccator. A second crop of precipitatewas obtainedonkeeping the filtrate for severalhours at 0C. Thecombined dried crops were purified by dissolving in a minimumof dry diethyl ether and adding dry petroleum ether (bp. 40-60C) at 0C. After 1 h at 0C, fine, very pale buff needles wereformed; these were filtered and dried in vacuo to give 1a (1.51 g,77%).

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, 4-Chloro-2-methoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Buglass, Alan J.; Datta, Mrityunjoy; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 193; 4; (2018); p. 218 – 224;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics