Tag: M.W=100-200

Synthetic Route of 108-70-3, 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. 108-70-3, name is 1,3,5-Trichlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

n-Butyllithium (2.45 mL, 4.00 mmol) was added to a tetrahydrofuran (10 mL) solution of 1,3,5-trichlorobenzene(724 mg, 4.00 mmol) at -78C in an argon atmosphere, and the mixture was stirred for 45 minutes.[0146] After the addition of dimethylformamide (0.31 mL, 4.00 mmol) at -78C, the mixture was stirred for 45 minutes.[0147] After increasing the temperature of the mixture to -20C, a saturated ammonium chloride solution (5 mL) wasadded to the mixture, followed by stirring for 5 minutes.[0148] The organic layer was extracted with ethyl acetate, dried over sodium sulfate, and filtered, and the solvent wasevaporated.[0149] The residue was purified by silica gel column chromatography (15 g, hexane_acetone=50:1 to 40:1) to obtaina 2,4,6-trichlorobenzaldehyde compound (colorless crystals) (633 mg, 76%).Reference: Synthesis, 2008, 279-285.

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, 1,3,5-Trichlorobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; National University Corporation University Of Toyama; MORI Hisashi; TOYOOKA Naoki; MIZUGUCHI Mineyuki; OBITA Takayuki; HIRONO Syuichi; GODA Hiroaki; EP2808014; (2014); A1;,
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Related Products of 1435-48-9,Some common heterocyclic compound, 1435-48-9, name is 2,4-Dichloro-1-fluorobenzene, molecular formula is C6H3Cl2F, 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.

448 mg of milled sodium hydroxide (1.4 eq; 0.0112 mmol), 1.32 g of 1,3-dichloro-4-fluorobenzene (1 eq; 0.008 mol) and 1.57 g of benzophenone hydrazone (1 eq; 0.008 mol) in 6 ml of degassed tert-amyl alcohol are loaded into a 20 ml reactor surmounted by a condenser, a mechanical stirrer and a temperature sensor, and placed in an inert atmosphere.8.95 mg of palladium acetate (0.001 mol %; 0.00004 mol) and 46.3 mg of 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (0.0008 mol) in 2 ml of degassed tert-amyl alcohol are loaded into a 100 ml Schlenk tube equipped with a magnetic stirrer and placed under an inert atmosphere.After stirring for twenty minutes, the catalyst thus prepared is transferred into the reactor.After stirring at 103 C. for 12 hours, the conversion of the 1,3-dichloro-4-fluorobenzene is complete and a benzophenone N-5-chloro-2-fluorophenylhydrazone yield of 85% (accompanied by 15% of benzophenone N-3-chloro-4-fluorophenylhydrazone) is measured by gas chromatography in the presence of an internal standard (hexacosane).

The synthetic route of 1435-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Rhodia Chimie; US7557248; (2009); B2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 2453-46-5, 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. 2453-46-5, name is Chlorocycloheptane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A 10 mL Schlenk tube was charged with CoBr2 (6.6 mg, 0.03mmol), 1,3-diisopropyl-1H-benzimidazol-3-ium bromide (L4; 8.5mg, 0.03 mmol), 4-methoxy-N-[(1E)-1-phenylethylidene]aniline(1a, 67.6 mg, 0.30 mmol), 1-chlorooctane (2a, 76.5 muL, 0.45 mmol), and THF (0.69 mL). A 1.92 M solution of t-BuCH2MgBr inTHF (0.31 mL, 0.60 mmol) was added dropwise at 0 C, and themixture was stirred at r.t. for 6 h. The reaction was quenched by theaddition of 3 M aq HCl (1.0 mL), and the mixture was stirred at r.t.for 1 h, then extracted with EtOAc (3 × 10 mL). The organic layerswere combined, dried (MgSO4), and concentrated under reduced pressure. The crude product was purified by chromatography [silicagel, hexane-EtOAc (40:1)].

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

Reference:
Article; Gao, Ke; Yamakawa, Takeshi; Yoshikai, Naohiko; Synthesis; vol. 46; 15; (2014); p. 2024 – 2039;,
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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. 1939-99-7, name is Phenylmethanesulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of Phenylmethanesulfonyl chloride

General procedure: Pyridine (73 lL, 0.90 mmol) and DMAP were added to a solution10a (203 mg, 0.7 mmol) in anhydrous DCM (10 mL). Then benzenesulfonylchloride (145 mg, 0.76 mmol) was dissolved in DCMand added dropwise under a nitrogen atmosphere. The reactionmixture was then stirred at room temperature for 1 day.Whereupon, HCl (1 mol/L) was added and the reaction mixturewas extracted with DCM. The organic phases were combined anddried over anhydrous Na2SO4. After removal of volatiles, a residuewas obtained that was then subjected to silica-gel column chromatographicpurification to afford this intermediate 13a (196 mg,63%).

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 1939-99-7.

Reference:
Article; Liu, Peihong; Du, Yongli; Song, Lianhua; Shen, Jingkang; Li, Qunyi; Bioorganic and Medicinal Chemistry; vol. 23; 21; (2015); p. 7079 – 7088;,
Chloride – Wikipedia,
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Application of 870-24-6, These common heterocyclic compound, 870-24-6, name is 2-Chloroethanamine 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.

AEA was synthesised according to the method described by Jung et al. [22]. 2-chloroethylamine hydrochloride (5 g, 43 mmol) was ground and dissolved in deionised water (50 ml). Sodium azide (8 g, 123 mmol) was added and the mixture was heated at 80 C for 18 h. The solution was then made alkaline with potassium hydroxide (15 g), extracted using diethyl ether and dried over magnesium sulphate. Finally the solution was concentrated using rotary evaporation to give an amber coloured, viscous oil. AEA was characterised using 1H NMR and FTIR spectroscopy (See Fig. S1, Supporting information). The integrations for the peaks gave the correct proton ratios and the FTIR spectra (Fig. 2(a)) showed a strong azide band at 2100 cm-1.

Statistics shows that 2-Chloroethanamine hydrochloride is playing an increasingly important role. we look forward to future research findings about 870-24-6.

Reference:
Article; Farley, Robert; Saunders, Brian R.; Polymer; vol. 55; 2; (2014); p. 471 – 480;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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 461-81-4 as follows. Computed Properties of C7H4ClF3O

a) Preparation of 4-trifluoromethoxybenzonitrile Process According to the Invention in MEK Under an atmosphere of nitrogen, a mixture of 6.5 g of bis-triphenylphosphine-nickel dichloride, 5 g of triphenylphosphine and 120 ml of MEK was stirred at room temperature for 10 minutes. 1.9 g of activated zinc powder were then added, and the reaction mixture was stirred at 70 C. for 30 minutes. Following this, the mixture was allowed to cool to 25 C., and 93.25 g of 1-chloro-4-trifluoromethoxybenzene were added dropwise. The mixture was stirred for 10 minutes, 24 g of sodium cyanide were added, and the reaction mixture was stirred at from 65 to 70 C. for 20 h. The conversion was then approximately 75% (GC). After cooling to room temperature, the mixture was filtered, the solid filter residue was washed 2* with 50 ml of MEK and the combined organic phases were concentrated under reduced pressure. Vacuum distillation gave 58.5 g (66% of theory) of 4-trifluoromethoxybenzonitrile as a colourless liquid (boiling point at 120 mbar: 80 C.). 2.6% of coupling products had formed.

According to the analysis of related databases, 461-81-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Bayer Aktiengesellschaft; US6162942; (2000); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 104-11-0, 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. 104-11-0, name is 1-(4-Chlorophenyl)-N-methylmethanamine, This compound has unique chemical properties. The synthetic route is as follows.

Example 111; N-(4-Chloro-benzyl)-2-(4-fluoro-phenyl)-N-methyl-4-[4-(2-oxo-pyrrolidin-1-yl)-piperidin-1-yl]-butyramide; a) Step 1; N-(4-Chloro-benzyl)-2-(4-fluoro-phenyl)-N-methyl-acetamide; A mixture of 1.09 g (7 mmol) 4-fluorophenylacetic acid, 1.37 g (9 mmol) (4-chloro-benzyl)-methyl-amine, 2.84 g (9 mmol) TBTU and 6 mL (35 mmol) DIPEA in 50 mL DMF was stirred at room temperature for 16 h. After evaporation of all volatiles Na2CO3 aq. was added and the mixture was extracted with ethyl acetate. The combined organic phases were washed with NaCl aq., dried with Na2SO4, filtered and evaporated to dryness. The residue was purified by column chromatography on silica eluting with a gradient formed from ethyl acetate and heptane. The product containing fractions were evaporated to yield 1.35 g (65%) of the title compound as yellow oil. MS(m/e): 292.2 (MH+).

The chemical industry reduces the impact on the environment during synthesis 1-(4-Chlorophenyl)-N-methylmethanamine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Knust, Henner; Nettekoven, Matthias; Ratni, Hasane; Vifian, Walter; Wu, Xihan; US2009/76081; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 452-83-5,Some common heterocyclic compound, 452-83-5, name is 2-Chloro-5-fluoroaniline, molecular formula is C6H5ClFN, 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: NaOt-Bu (0.240 g, 2.5 mmol), Pd(OAc)2 (0.006 g, 0.025 mmol) and [HPt-Bu3][BF4] (0.010 g, 0.035 mmol) were suspended in toluene (3 ml) in a 5 ml microwave vial. The appropriate 2-chloroaniline (0.50 mmol) and aryl bromide (0.50 mmol) were then added and the vial sealed. The reaction was then heated in the microwave reactor at 160 C for 3 h, allowed to cool, and then quenched by addition of aqueous HCl (2 M, 3 ml). The organic phase was extracted with CH2Cl2 (2×20 ml), dried (MgSO4), then filtered and the solvent removed under reduced pressure. The crude product mixture was then subjected to column chromatography (SiO2).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-5-fluoroaniline, its application will become more common.

Reference:
Article; Bedford, Robin B.; Bowen, John G.; Weeks, Amanda L.; Tetrahedron; vol. 69; 22; (2013); p. 4389 – 4394;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 108-70-3, name is 1,3,5-Trichlorobenzene, 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 108-70-3, Application In Synthesis of 1,3,5-Trichlorobenzene

Step 2: Preparation of (3,5-dichloro-4-pyridinyl)bis(2,4,6-trichlorophenyl)methane A 100 mL round-bottom flask was charged with 3,5-dichloropyridine-4-aldehye (1.76 g, 10.0 mmol), 1,3,5-trichlorobenzene (18.14 g, 100 mmol) and trifluoromethanesulphonic acid (30.0 g, 200 mmol) and heated to 180 C. for 10 h. After the reaction was completed and cooled to room temperature, the mixture was dissolved with dichloromethane and added to ice water. The mixture was neutralized to pH 7 using saturated sodium hydrogen carbonate solution, extracted with dichloromethane, washed with a sodium hydrogen carbonate solution several times, dried over magnesium sulphate. The solvent was evaporated under the reduced pressure. Product was purified by silica gel chromatography eluting with petroleum ether:methylene dichloride=1:1 (VV). A white solid (2.6 g, 50%) was obtained. 1H NMR and mass spectrometry results confirmed that product was (3,5-dichloro-4-pyridine)bis(2,4,6-trichlorophenyl)methane.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,3,5-Trichlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; JILIN UNIVERSITY; LI, Feng; (18 pag.)US2016/99415; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 622-86-6, 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. 622-86-6 name is (2-Chloroethoxy)benzene, 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.

The synthesis of Intermediates 8, 9 and 10 was carried out according to Hardcastle et al. (1995) and is shown in Scheme II.The mixture containing the tamoxifen precursor Intermediate 10 obtained after column chromatography was dried under high vacuum and minimum volume of absolute ethanol was added to dissolve it. It was heated to boiling and then transferred to the freezer at 0 0C. After 2 hrs it was brought out of the freezer and kept at room temperature. The sudden temperature difference makes the E- isomer to precipitate as fluffy white crystals that should be kept under constant supervision so as to filter the crystals off at the right moment before the Z-isomer also starts that has to be followed by 1H NMR of the precipitated crystals. EPO Sometimes the crystals of E-isomer also start falling out when it is in the freezer, thus the solution should be continuously monitored so that after the initiation of the crystallization process it can be brought out of the freezer and kept at room temperature. The total time taken for crystallization varies depending on the room temperature. At 30 C it takes about 2-3 hrs and at low room temperature it may take 10-12 hours. Thus, it is preferable to heat the room at 30 0C for faster and efficient crystallization.

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

Reference:
Patent; YEDA RESEARCH AND DEVELOPMENT CO. LTD.; WO2006/80022; (2006); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics