Tag: M.W=100-200

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 67330-62-5 as follows. Quality Control of 3-Chloro-2,6-diethylaniline

A mixture of 7-hydroxynaphthalene- 1,3 -disulfonyl dichloride (255 mg, 0.75 mmol) and 2,6-diethylaniline (550 mg, 3.0 mmol) in acetonitrile (3 mL) was heated under reflux during 4 h. The reaction mixture was diluted with water (30 mL) and extracted with ethyl acetate (30 mL). The extract was washed with 4% HCl (30 mL), dried with Na2SO4, evaporated and purified by chromatography (petroleum ether- ethylacetate, 2:1). Yield 21 mg (4%), as a white powder, mp 142-144 C.1H NMR (DMSO-^), delta: 0.75-0.98 (m, 12H); 2.05-2.46 (m, 8H); 7.09 (dd, J = 8.4,2.1 Hz5 2H); 7.32 (d, J = 8.4 Hz5 2H); 7.38 (dd, J= 9.0, 2.2 Hz5 IH); 7.94 (d, J =2.2 Hz5 IH); 8.19 (d, J = 9.1 Hz, IH); 8.28 (d, J= 1.9 Hz, IH); 8.45 (d, J = 1.9 Hz, IH); 9.78 (s, IH); 10.01 (s, IH); 10.65 (s, IH).

According to the analysis of related databases, 67330-62-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BIOLIPOX AB; WO2007/42817; (2007); A1;,
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. 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C3H4Cl3NO

General procedure: Preparation of 2-methyl-6-nitro-2H-indazole (5d). To a stirred mixture of 6-nitro-1H-indazole (1.0 g, 0.0061 mmol) in dichloromethane (25.0 mL) was added trifluoromethanesulfonic acid (0.54 mL, 0.0061 mmol), stirred for 5-10 min at 25-35 C. To this mixture was added methyl 2,2,2,-trichlroacetimidate (2.69 g, 0.015 mmol) at room temperature. The reaction mixture was stirred at room temperature for 16-18 h under N2. After reaction completion, chilled saturated NaHCO3 solution was added. The aqueous and organic phases were separated. Aqueous phase was extracted with dichloromethane 10 mL. Combined organic layers were washed with DM water (2 × 10 mL). Organic layer was dried over anhydrous Na2SO4, filtered, and evaporated completely under vacuum to obtain 2-methyl-6-nitro-2H-indazole (1.03 g, 95.0%) as a yellow solid.

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 2533-69-9.

Reference:
Article; Baddam, Sudhakar Reddy; Uday Kumar; Panasa Reddy; Bandichhor, Rakeshwar; Tetrahedron Letters; vol. 54; 13; (2013); p. 1661 – 1663;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

1303587-99-6, name is 2-Chloro-7,8-dihydro-6H-pyrimido[5,4-b][1,4]oxazine, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 2-Chloro-7,8-dihydro-6H-pyrimido[5,4-b][1,4]oxazine

Synthesis of 2-chloro-8-(4-fluorobenzyl)-7 , 8-dihydro-6H-pyrimido [5, 4-b] [I, 4] oxazine [0440] To a stirred solution of 2-chloro-7, 8-dihydro-6H-pyrimido [5, 4-b] [1, 4] oxazine (100 mg, 0.58 mmol) in DMF (1 mL) under argon atmosphere was added sodium hydride (27 mg, 1.16 mmol) at 0 C. After stirring for 10 mins, l-(bromomethyl)-4-fluorobenzene (132 mg, 0.70 mmol) was added at 0 C and stirred for 1 h. After consumption of the starting materials (monitored by TLC), the reaction was quenched with ice water (20 mL) and extracted with EtOAc (2 x 20 mL). The combined organic extracts were dried over sodium sulfate, filtered and concentrated in vacuo to afford 2-chloro-8-(4-fluorobenzyl)-7, 8-dihydro- 6H-pyrimido [5, 4-b] [1, 4] oxazine (150 mg, 92%) as an off-white solid. 1H-NMR (DMSO- d6, 400 MHz): delta 7.70 (s, 1H), 7.36 (t, 2H), 7.18 (t, 2H), 4.75 (s, 2H), 4.19-4.16 (m, 2H), 3.51- 3.48 (m, 2H); LCMS: 279.9 (M+1); (column; X-Select CSH C-18 (50 3.0 mm, 3.5 mupiiota); RT 3.59 min 0.05% Aq TFA: ACN; 0.80 mL/min); TLC: 60% EtOAc/hexane (R 0.5).

The synthetic route of 1303587-99-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FORUM PHARMACEUTICALS INC.; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; MCRINER, Andrew, J.; WO2015/66697; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 6940-78-9, 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. 6940-78-9, name is 1-Bromo-4-chlorobutane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 9; Preparation 7-CBQ by a Reaction of 7-HQ with 1-bromo-4-chlorobutane in 2-propanol in Presence of About 47% sodium hydroxide solution; A mixture of 7-hydroxy-3,4-dihydro-2(1H)-quinolinone (4 g, 0.024 mole) and 1-bromo-4-chlorobutane (8.6 ml, 12.75 g, 0.073 mole, 3 eq.) in 2-propanol (20 ml) was refluxed followed by addition of mixture of about 47% aqueous sodium hydroxide solution (2.5 g, 0.029 mole, 1.2 eq.) and 2-propanol (4 ml). Reflux was continued for 2 hours. The hot reaction mixture was filtered, and the solvent and an excess of 1-bromo-4-chlorobutane were removed to dryness in vacuum. 2-propanol (12.5 ml) was added to the residue thus obtained and the mixture was refluxed to obtain a solution, followed by addition of a solution of 47% aqueous sodium hydroxide to produce a pH of about 10-11. The mixture was set aside at 10-15 C. for 6 hours. A colorless precipitate was collected by filtration, washed with cold mixture of water and 2-propanol (1:3, 7 ml) and water (10 ml). The solid was dried under reduced pressure at 50 C. overnight to obtain 7-(4-chlorobutoxy)-3,4-dihydro-2(1H)-quinolinone (5.55 g) in 89.2% yield, having a purity of 98.2% (by HPLC).

The synthetic route of 1-Bromo-4-chlorobutane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Naddaka, Vladimir; Brand, Michael; Davidi, Guy; Klopfer, Eyal; Gribun, Irina; Arad, Oded; Kaspi, Joseph; US2006/79689; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 363-51-9, 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. 363-51-9 name is 2-Chloro-6-fluoroaniline, This 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 2-chloro-6-fluoroaniline (24.8 g, 165 mmol) in HOAc (90 mL) is added Ac2O (18 mL, 189 mmol) and the mixture is stirred at 90 C. for 1 h. After cooling to rt H2O is added and the mixture is neutralized with 2 M NaOH solution with stirring. The aqueous layer is extracted twice with DCM. The combined organic layer is washed with semi-saturated NaHCO3 solution and brine, dried over MgSO4 and evaporated to give the acetanilide which is used without further purification

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-6-fluoroaniline, and friends who are interested can also refer to it.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2012/322803; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 102-49-8, name is 3,4-Dichlorobenzylamine, 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 102-49-8, Application In Synthesis of 3,4-Dichlorobenzylamine

A mixture of 3,4-dichlorobenzylamine (440 mg, 2.5 mmol) and acrylimide (185 mg, 2.6 mmol) was treated with silicon tetrachloride (6 mul, 0.05 mmol) under solvent-free conditions at 0°C. The mixture was heated to 60°C and stirred for 4 hr. The reaction was allowed to cool to rt and ethyl acetate (20 mL) and water (20 mL) were added. The layers were separated and the aqueous layer was further extracted with ethyl acetate (2 x 20 mL) and the combined organic layers were dried over sodium sulfate and concentrated in vacuo. The crude product was purified by flash column chromatography eluting with a gradient of dichloromethane: methanol (95:5 ? 85:15) to yield the product as a white solid (378 mg, 61percent).

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, 3,4-Dichlorobenzylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Brear, Paul; North, Andrew; Iegre, Jessica; Hadje Georgiou, Kathy; Lubin, Alexandra; Carro, Laura; Green, William; Sore, Hannah F.; Hyvoenen, Marko; Spring, David R.; Bioorganic and Medicinal Chemistry; vol. 26; 11; (2018); p. 3016 – 3020;,
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. 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, This compound has unique chemical properties. The synthetic route is as follows., Safety of Methyl 2,2,2-trichloroacetimidate

500 mg (2.31 mmol) 3,4-diamino-benzene-sulfonylethan-2-ol were dissolved in 10 ml concentrated acetic acid. 0.4 ml (1.4 equiv.) methyl-2,2,2-trichloroacetimidate were added slowly and the resulting mixture was stirred at room temperature for 4 h. The mixture was diluted with 100 ml toluene and the solvent was removed under reduced pressure. The residue was rinsed with toluene, filtered and dried under vacuo to give a brown crystalline solid pure enough for all further reactions. Yield: 680 mg MS (ES+): m/e = 345, chloro pattern.

According to the analysis of related databases, 2533-69-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Aventis Pharma Deutschland GmbH; EP1479676; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2401-24-3, name is 2-Chloro-5-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 2401-24-3, COA of Formula: C7H8ClNO

To a solution of 2-chloro-5-methoxyaniline (500 mg) and TEA (0.49 mL) in MeCN (4 mL) was added phenylacetyl chloride (0.42 mL) at 0 C., and the mixture was stirred at room temperature for 30 minutes. To the reaction solution was added water, and the mixture was extracted with AcOEt and washed with brine. The organic layer was dried over anhydrous sodium sulfate, and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (Hexane/AcOEt) to give N-(2-chloro-5-methoxyphenyl)-2-phenylacetamide (657 mg).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloro-5-methoxyaniline, and friends who are interested can also refer to it.

Reference:
Patent; OTSUKA PHARMACEUTICAL CO., LTD.; KAWANO, Yoshikazu; SHIMIZU, Hiroshi; ISHIKAWA, Shunpei; TAKEMURA, Isso; HARIGUCHI, Norimitsu; MATSUBA, Miki; MATSUMOTO, Makoto; (92 pag.)US2019/40039; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 29671-92-9, name is Carbamimidic chloride hydrochloride, 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. Safety of Carbamimidic chloride hydrochloride

A suspension of 3-amino-benzo[b]thiophene-2-carboxylic acid methyl ester (1.03 g, 5.0 mmol) and chloroformamidine hydrochloride (800 mg, 7.0 mmol) in diglyme (8 mL) were heated at 160 C. for 1 h. The resulting suspension was cooled to rt and filtered, and the collected solid was suction dried to give the title compound (1.14 g, 90%). 1H NMR (DMSO-d6): 8.06 (d, J=7.9 Hz, 1H), 7.89 (d, J=8.1 Hz, 1H), 7.73-7.47 (m, 2H), 7.45-7.39 (m, 1H), 7.38-7.33 (m, 1H), 7.18 (s, 0.6H), 7.05 (s, 0.6H), 6.92 (s, 0.6H).

The synthetic route of Carbamimidic chloride hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chavez, Frank; Curtis, Michael P.; Edwards, James P.; Gomez, Laurent; Grice, Cheryl A.; Kearney, Aaron M.; Savall, Brad M.; US2008/15200; (2008); 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. 98446-49-2, name is 2,4-Dichloro-5-methoxyaniline, A new synthetic method of this compound is introduced below., Computed Properties of C7H7Cl2NO

A mixture of 6-butoxy-4-chloro-7-(2-methoxyethoxy)-3-quinolinecarbonitrile (184 mg, 0.55 mmol), 2,4-dichloro-5-methoxyaniline (127 mg, 0.66 mmol) and pyridine hydrochloride (76 mg, 0.66 mmol) in 5 mL of 2-ethoxyethanol is heated at 120 C. for 7 hours. The reaction mixture is cooled to room temperature and concentrated in vacuo. Diethyl ether is added to the residue and the solids are collected and suspended in saturated aqueous sodium bicarbonate. After stirring for 1 hour the solids are collected by filtration and washed with water. Purification by preparatory thin layer chromatography, eluting with 7% methanol in dichloromethane provides 93 mg of 6-butoxy-4-[(2,4-dichloro-5-methoxyphenyl)amino]-7-(2-methoxyethoxy)-3-quinolinecarbonitrile, mp 166-167 C. [0494] MS 488.0 (M-H)-[0495] Analysis for C24H25Cl2N3O4-0.5 H2O [0496] Calcd: C, 57.72; H, 5.25; N, 8.41. [0497] Found: C, 57.67; H, 4.93; N, 8.49.

The synthetic route of 98446-49-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Wyeth Holdings Corporation; US2003/212276; (2003); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics