Author: Jessica.F

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. 106131-61-7, name is 3,6-Dichloro-1,2,4,5-tetrazine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 106131-61-7

To a solution of 3,6-dichloro-1,2,4,5-tetrazine (1.51 g, 10 mmol) in acetonitrile (70 ml) was added the sodium salt of 5-amino-1H-tetrazole (2.14 g, 10 mmol). The mixture was refluxed for 24 hours then allowed to cool to room temperature. The suspension was centrifuged until the supernatant liquid was clear. The liquid was decanted and the brown solid washed successively with acetonitrile and water. With each wash the solid was separated from the solvent by centrifugation followed by decantation. The isolated crude yield was 1.5 g (60%), this material was recrystallized from DMSO/methanol yielding an orange brown powder mp 264 C. dec; 1H NMR(deuteriomethylsulfoxide) 12.5(b,r s,4H); 13 C NMR (deuteriomethylsulfoxide) 151.74, 158.25; IR (KBr) 3421, 3000, 1615, 1436, 1127 cm-1. A gas pycnometer density of 1.76 g/cm3 was also determined and a drop height of 195 cm was measured (Type 12, HMX=24-27 cm).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 106131-61-7.

Reference:
Patent; The Regents of the University of California; US6657059; (2003); B2;,
Chloride – Wikipedia,
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Some common heterocyclic compound, 4535-90-4, name is 2-Chloro-N-methylethanamine hydrochloride, molecular formula is C3H9Cl2N, 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. Recommanded Product: 2-Chloro-N-methylethanamine hydrochloride

A mixture of tra/75-8-chloro-l-[4-(5-methyl-isoxazol-3-yl)-cyclohexyl]-5,6-dihydro-4H- 2,3,5, 10b-tetraaza-benzo[e]azulene (50.0 mg, 0.130 mmol), cesium carbonate (170 mg, 0.521 mmol) and 2-methylaminoethyl chloride hydrochloride (67.7 mg, 0.521 mmol) in acetonitrile (1.3 ml) was heated at 70 C for 20 h. After cooling to room temperature the reaction mixture was partitioned between 1 M aqueous sodium hydroxide solution (2 ml) and ethyl acetate (5 ml). The layers were separated. The aqueous layer was extracted with three 5-ml portions of ethyl acetate. The combined organic layers were concentrated in vacuo. Preparative RP-HPLC with water (0.05% formic acid) / methanol as eluent gave the hydro formate salt of the title compound, which was liberated by filtration over aminopropyl modified silica gel (10 g) with methanol (20 ml) as eluent. The filtrate was concentrated to dryness. The residue was redissolved in ethyl acetate, filtrated over cotton wool and concentrated to dryness to give the title compound (38 mg, 66%) as off-white solid. MS m/e: 441 ([M+H]+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4535-90-4, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; DOLENTE, Cosimo; SCHNIDER, Patrick; WO2011/141396; (2011); A1;,
Chloride – Wikipedia,
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Reference of 1996-30-1, 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. 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

[00227] Step 12. 3-Bromo-5-chloro-2-fluorobenzaldehyde. A solution of 2,2,6,6- tetramethylpiperidine (327 g, 98%, 2.274 mol) and THF (1.9 L, HPLC grade) was cooled to -75 0C (dry ice-methanol bath) under an argon atmosphere. 1.6 M n-BuLi/hexane solution (1.47 L, 2.35 mol) was added slowly into the mixture at -72 to -67 0C over 1 h. The mixture was stirred at -72 to -67 0C for 30 min to give a pale yellow suspension. 2-Bromo-4-chloro-l-fluorobenzene (435 g, 97%, 2.02 mol) was added slowly into the mixture at -72 to -67 0C over 30 min, and then the mixture was stirred at -72 to -67 0C for an additional 30 min. Dimethylformamide (230 g, 99.5%, 3.14 mol) was added slowly into the mixture at -70 to -65 0C over 30 min and then the mixture was stirred at -70 to -65 0C for 30 min to afford a light brown solution. The cooling bath was removed and then saturated ammonium chloride solution (720 mL) was added into the batch at -60 to -30 0C over 15 min to obtain a hazy mixture. 6 N hydrochloric acid was quickly added into the mixture at -30 to 10 0C over 15 min to pH 1 and then ethyl acetate (2.0 L) was added at 10 to 20 0C. The layers were separated and the aqueous layer was extracted with ethyl acetate (1 x 300 mL). The combined organic extracts were washed with water (I x 800 mL) and brine (I x 500 mL), dried over magnesium sulfate, and filtered. The filtrate was concentrated under vacuum (60-65 0C) to give the title compound as a tan viscous oil, which solidified upon standing after several hours. 1H NMR (CDCl3): delta 7.76-8.30 (m, 2H), 10.0-10.8 (br s, IH); MS m/z 238.0 (M+l).

The synthetic route of 3-Bromo-4-fluorochlorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IRM LLC; NOVARTIS AG; HUANG, Shenlin; JIN, Xianming; LIU, Zuosheng; POON, Daniel; TELLEW, John; WAN, Yongqin; WANG, Xing; XIE, Yongping; WO2011/25927; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 84859-27-8, The chemical industry reduces the impact on the environment during synthesis 84859-27-8, name is 5-Chloro-N1-methylbenzene-1,2-diamine, I believe this compound will play a more active role in future production and life.

General procedure: General procedure for the synthesis of 2-mercaptobenzimidazole derivatives (18-34): the proper 1,2-phenylenediamine 1-17 (16 mmol) was added over a stirred solution of ethanol (50 mL), water (5 mL), potassium hydroxide (19.2 mmol) and carbon disulfide (19.2 mmol). The mixture was heated overnight under a N2 atmosphere at 50 C. The cold reaction mixture was then neutralized with acetic acid and poured into 250 mL of cold water for complete precipitation. The solid was separated and dried using vacuum filtration. The crude product was purified by recrystallization, adding norite to the solvent.

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, 5-Chloro-N1-methylbenzene-1,2-diamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Perez-Villanueva, Jaime; Hernandez-Campos, Alicia; Yepez-Mulia, Lilian; Mendez-Cuesta, Carlos; Mendez-Lucio, Oscar; Hernandez-Luis, Francisco; Castillo, Rafael; Bioorganic and Medicinal Chemistry Letters; vol. 23; 14; (2013); p. 4221 – 4224;,
Chloride – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 367-22-6, name is 4-Chloro-3-fluoroaniline, 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 367-22-6, Computed Properties of C6H5ClFN

To 4-chloro-3-fluoroaniline (25g, 0.17 mmol) in 250 mL of H2O was added NaHCO3 (21.6g, 0.25 mmol). After cooling to 0 C, iodine (43.5 g, 0.17 mmol) was added. After 18 h at rt, an additional 10.8 g of iodine was added and the reaction was stirred overnight. The reaction was extracted with DCM (4×250 mL), the combined organics were washed with sodium thiosulfate solution (2×250 mL) and brine (2×250 mL) and dried (Na2SO4). Purification by silica gel chromatography gave 47 g of Intermediate 5A. MS (ESI) m/z: 145.2 (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, 4-Chloro-3-fluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ORWAT, Michael J.; PINTO, Donald J.P.; SMITH II, Leon M.; SRIVASTAVA, Shefali; WO2013/56060; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 60811-21-4,Some common heterocyclic compound, 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, molecular formula is C6H3BrClF, 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.

Step 1: tert-Butyl 4-(3-chloro-4-fluorophenyl)piperazine-1-carboxylate A solution of tert-butyl-piperazine-1-carboxylate (1.0 g, 5.37 mmol), 4-bromo-2-chloro-1-fluorobenzene (1.35 g, 6.44 mmol), t-BuONa (768 mg, 8.06 mmol), BINAP (125 mg, 0.2 mmol), Pd2(dba)3 (92 mg, 0.1 mmol) in dry toluene (10 mL) was stirred under N2 at 80 C. for 16 hrs. The reaction mixture was concentrated and the mixture was purified by chromatography (silica, EtOAc/PE=1/10) to afford tert-butyl-4-(3-chloro-4-fluorophenyl)piperazine-1-carboxylate (1.3 g, 4.13 mmol, 77%) as a yellow oil. ESI-MS (EI+, m/z): 259 [M-55]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Bromo-2-chloro-1-fluorobenzene, its application will become more common.

Reference:
Patent; Navitor Pharmaceuticals, Inc.; O’Neill, David John; Saiah, Eddine; Kang, Seong Woo Anthony; Brearley, Andrew; Bentley, Jonathan; (136 pag.)US2019/389843; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 41965-95-1, 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. 41965-95-1, name is 3-Chloro-4-methoxybenzylamine Hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 2 (1.92 mmol), 3-chloro-4-methoxybenzylamine hydrochloride (2.11 mmol), NaI (0.1 mmol), and phenol (3.84 mmol) was heated at 130 C. for 1.5 h. After cooling the reaction down, Et2O (20 mL) was added and washed with 1N NaOH (3¡Á20 mL). The organic layer was dried over Na2SO4, filtered and evaporated under reduced pressure. The residue was purified by Flash Chromatography (AcOEt:MeOH 8:2) to give the desired compound A (38% yield). 1H NMR (300 MHz, CDCl3) delta 8.04 (d, 1H, J=2.1 Hz), 7.80 (d, 1H, J=8.7 Hz), 7.64 (dd, 1H, J1=2.1, J2=9.0 Hz), 7.38 (d, 1H, J=2.1 Hz), 7.16 (dd, 1H, J1=2.1, J2=8.4 Hz), 6.91 (d, 1H, J=8.4 Hz), 4.47 (d, 2H, J=5.7 Hz), 3.91 (s, 3H), 3.54 (s, 2H), 3.18 (t, 2H, J=6.3 Hz), 2.81 (t, 2H, J=6.3 Hz), 2.50 (s, 3H).

The synthetic route of 3-Chloro-4-methoxybenzylamine Hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; Landry, Donald W.; Deng, Shixian; Arancio, Ottavio; Fiorito, Jole; Wasmuth, Andrew; (41 pag.)US10626113; (2020); B2;,
Chloride – Wikipedia,
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These common heterocyclic compound, 16793-91-2, name is 2-Chlorophenethyl Bromide, 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. Quality Control of 2-Chlorophenethyl Bromide

EXAMPLE 1 Preparation of 1-(2-chlorophenyl)-3-(4-pyridyl)-butane In a 200-ml flask, 0.94g (9.35 mmol) of diisopropyl amine and 15 ml of tetrahydrofuran were placed and cooled to -50 C. Then 6.5 ml (10.3 mmol) of n-butyl lithium (15% n-hexane solution) was added thereto under nitrogen atmosphere. The resulting mixture was stirred for 10 minutes, and a solution of 1.0 g (9.35 mmol) of 4-ethylpyridine dissolved in tetrahydrofuran was added dropwise. After stirring for 30 minutes at -50 C., the reaction temperature was gradually raised up to -10 C., which was kept for 30 minutes, and lowered again to -50 C. A solution of 2.05 g (9.35 mmol) of 2-chlorophenethyl bromide dissolved in tetrahydrofuran was added dropwise to the reaction mixture, and after stirring for 30 minutes at -50 C., the temperature was raised up to room temperature. Subsequently, water was added, tetrahydrofuran was distilled away under reduced pressure, and the residue was extracted with ethyl acetate. The extract was washed with saturated brine, then dried over anhydrous sodium sulfate. Then, the solvent was distilled away under reduced pressure, to obtain an oil. Said oil was purified by silica gel column chromatography, to obtain 1.35 g of the desired compound (yield: 58.2%). The resulting compound was identified as 1-(2-chlorophenyl)-3-(4-pyridyl)-butane (hereinafter referred to as compound 1) by melting point, infrared ray absorption spectrum (IR), nuclear magnetic resonance spectrum (NMR) and elementary analysis.

The synthetic route of 2-Chlorophenethyl Bromide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; US5262420; (1993); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 13726-14-2, name is 4-Chloro-3-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 13726-14-2, Recommanded Product: 13726-14-2

A mixture of ethyl 2,4-dichloropyrimidine-5-carboxylate (0.442 g, 2.0 mmol), 4-chloro-3- methoxyaniline (0.331 g, 2.1 mmol), DIPEA (0.42 mL, 2.4 mmol), and iPrOH (2 mL) was added to a 5 mL microwave vial which was then sealed and placed in a hot oil bath with stirring at 85 C overnight for 17 hours. At this point, a brown solid had formed and this was then washed with iPrOH (10 mL), water (10 mL), iPrOH (10 mL), and hexanes (10 mL) to yield RJ1-061 as a brown solid (0.570 g, 83%). m.p. = 119 C (decomposed). NMR (400 MHz, DMSO-ifc) delta 10.27 (s, 1H), 8.81 (s, 1H), 7.48 (d, / = 2.3 Hz, 1H), 7.43 (d, / = 8.6 Hz, 1H), 7.28 (dd, / = 8.6, 2.3 Hz, 1H), 4.37 (q, / = 7.1 Hz, 2H), 3.85 (s, 3H), 1.34 (t, / = 7.1 Hz, 3H). LRMS (ESI+) m/z 342.1 (MC135C135+H)+, 344.0 (MC135C137+H)+, 346.0 (MC137C137+H)+; (ESI-) m/z 339.3 (MC135C135-H)-; HRMS (ESI+) m/z calculated for C14H13CI2N3O3 (M+H)+ 342.04067, found 342.04100.

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.

Reference:
Patent; H. LEE MOFFITT CANCER CENTER & RESEARCH INSTITUTE, INC.; SCHOeNBRUNN, Ernst; LAWRENCE, Nicholas J.; LAWRENCE, Harshani R.; (293 pag.)WO2017/66428; (2017); A1;,
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. 2687-12-9, name is Cinnamyl chloride, A new synthetic method of this compound is introduced below., Safety of Cinnamyl chloride

To a solution of 2.94 g (0.02 mol) of isatin in 20 mL of DMF with stirring at 10C was slowly added 0.84 g (0.02 mol) of sodium hydride (60% suspension in mineral oil). After 30 min, 2.92 mL (0.02 mol) of cinnamyl chloride was added to the resulting purple solution followed by stirring at room temperature for 3 h. The reaction mixture was poured into 100 g of crushed ice. Next, the resulting precipitate was filtered off, washed with hexane, and dried in a vacuum(18 mmHg).

The synthetic route of 2687-12-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Bogdanov; Sadykov; Musin; Khamatgalimov; Krivolapov; Dobrynin; Mironov; Russian Journal of General Chemistry; vol. 85; 9; (2015); p. 2030 – 2036; Zh. Obshch. Khim.; vol. 85; 9; (2015); p. 1446 – 1452,7;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics