Tag: M.W=100-200

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.

a) 2-Chloro-5-fluorobenzenesulfonyl chloride 5 g (34.3 mM) of 2-chloro-5-fluoroaniline were slowly added to a solution of 17 ml of concentrated hydrochloric acid solution and 11 ml of water at 0 C. The reaction mixture is stirred at 0 C. for 1 hour. Addition of 2.49 g (36.1 mM) of NaNO2 in 6 ml of H2O is followed by stirring the mixture at 0 C. for 15 minutes and then adding to a solution of 692 mg (5.15 mM) of sulfur dioxide and copper(II) chloride in 10 ml of acetic acid. The reactants were stirred at 0 C. for 15 minutes and then at room temperature for a further 15 minutes. The reaction mixture is extracted with EtOAc. The organic phase is concentrated, dissolved in EtOAc, washed with 1N NaHCO3 solution, dried over MgSO4 and concentrated. 7.86 g of the desired sulfonyl chloride are obtained as a yellow oil.

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:
Patent; SANOFI-AVENTIS DEUTSCHLAND GMBH; US2007/197539; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1939-99-7, 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. 1939-99-7, name is Phenylmethanesulfonyl chloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A solution of phenylmethanesulfonyl chloride (2.19 g, 10 mmol) was added into a suspension of 3-bromopropan-1-amine hydrobromide (2.19 g, 10 mmol) and Et3N (2.02 g, 20 mmol) in THF (50 mL) at 0 C. The mixture was stirred at 0 C. for 5 min. TLC confirmed the completion of reaction. Solid was filtered out with suction, and the filtrate was concentrated to provide compound N-(3-bromopropyl)(phenyl)methanesulfonamide (2.7 g, quant.) as a pale yellow solid which was used in the next step without further purification. 1H NMR (300 MHz, CDCl3) delta 7.40 (m, 5H), 4.48 (m, 1H), 4.27 (s, 2H), 3.41 (t, J=6.6 Hz, 2H), 3.16 (q, 2H), 2.01 (m, 2H). LCMS (ESI), m/z, 314 and 316 [M+Na]+, Br pattern found.

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

Reference:
Patent; Genentech, Inc.; Fauber, Benjamin; Gobbi, Alberto; Rene, Olivier; van Niel, Monique Bodil; Gancia, Emanuela; Gaines, Simon; Ladduwahetty, Tammy; Vesey, David; Ward, Stuart; Winship, Paul; (101 pag.)US2016/168141; (2016); A1;,
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Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 83121-15-7, These common heterocyclic compound, 83121-15-7, name is 3,5-Dichloro-2,4-difluoroaniline, 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.

c. Preparation of 2,4-difluoro-1,3,5-trichlorobenzene 31.1 g of 3,5-dichloro-2,4-difluoroaniline (0.157 mol) was added to 100 ml of a solution of concentrated hydrochloric acid and water (1:1) at 70 C. The resulting mixture was stirred to be a slurry and cooled to 0-5 C. To the mixture was added 11.6 g of aqueous solution of sodium nitrite (0.165 mol) over 30 minutes. The resulting solution was added to a solution of CuCl (0.188 mol) and hydrochloric acid (100 ml). The reaction mixture was stirred for 2 hours and kept overnight. Fractions obtained by wet-distillation were extracted with toluene. The extract was washed successively with 10% aqueous solution of NaOH, concentrated sulfuric acid and water, dried over sodium sulfate and evaporated. The residue was recrystallized from toluene to give 27.7 g of 2,4-difluoro-1,3,5-trichlorobenzene (0.127 mol) in 81.1% yield.

Statistics shows that 3,5-Dichloro-2,4-difluoroaniline is playing an increasingly important role. we look forward to future research findings about 83121-15-7.

Reference:
Patent; Wang, Yuncai; Chen, Rongye; Nan, Haijun; US2003/166936; (2003); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, 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 2533-69-9, Formula: C3H4Cl3NO

REFERENTIAL EXAMPLE 17 4-Amino-7-fluoro-3-(trichloroacetimidoylamino)quinoline diacetate (VIII-1) STR146 To a solution of 1.77 g of 3,4-diamino-7-fluoro-quinoline (V-4) in 20 ml of acetic acid was added 1.94 g of methyl trichloroacetimidate and the mixture was stirred for two hours at room temperature. After concentration under reduced pressure, 10 ml of ethyl acetate was added to the residue, and the mixture was allowed to stand overnight. The crystals precipitated were collected by filtration and washed with ethyl acetate and then a small quantity of ethanol to give 3.75 g (yield: 87%) of the titled compound (VIII-1).

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; Shionogi & Co., Ltd.; US4940714; (1990); 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. 6940-78-9, name is 1-Bromo-4-chlorobutane, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H8BrCl

31 g of NaH (1.292 mol) was dissolved in 140 ml of DMF in batches under nitrogen blanket and ice bath.Weigh out 3-methyl-6-azauracil 14g (0.110mol),Dissolved in DMF in batches,After stirring for 1 hour,Add 1-bromo-4-chlorobutane 20g,The reaction continued overnight at room temperature.The reaction mixture was then added to ice water and extracted twice with EA.The combined organic phases were washed with brine.It was dried over anhydrous sodium sulfate and concentrated.The residue was purified by silica gel column chromatography.Obtaining a solid product2-(4-Chlorobutyl)-4-methyl-1,2,4-triazin-3,5(2H,4H)-dione (CD-5)9g (0.041mol, yield: 72%)

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Central South University; Zhong Shian; Peng Wei; Chen Jian; Liu Hui; Li Xiufang; Li Jianbing; Tang Rongdi; (16 pag.)CN108440505; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine, 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. SDS of cas: 918538-05-3

101A. 2,4-dichloropyrrolo[1,2-f][1,2,4]triazine-7-carbaldehyde Dry dimethylformamide (1.03 mL, 13.3 mmole) was added to an ice-cooled solution of phosphorous oxychloride (2.47 mL, 26.6 mmole) in a vial and the mixture was stirred until homogeneous. It was allowed to warm to room temperature and 2,4-dichloropyrrolo[1,2-f][1,2,4]triazine 1B (500 mg, 2.66 mmole) was added and the vial was sealed and heated at 95 C. for 5 hr. After cooling to RT, the reaction was slowly poured into an ice-cooled, stirred mixture of saturated aqueous solution of NaHCO3 (75 mL) and dichloromethane (25 mL). The aqueous phase was separated and extracted with additional dichloromethane. The combined organic phases were dried (Na2SO4) and the solvent removed. Radial silica gel chromatography (elution with mixtures of DCM_hexane=1:1 followed by 3:1) afforded the product as a solid (371 mg, 65% yield): 1H NMR (CDCl3) delta 7.08 (d, 1H, J=5 Hz), 7.54 (d, 1H, J=5 Hz), 10.49 (s, 1H).

The synthetic route of 918538-05-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2008/9497; (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. 772-49-6, name is 1-Chloro-3-(trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

To a cooed (-78 C) soution of 1-choro-3-(trifluoromethoxy)benzene (100 g, 510 mmo)in THF (500 mL) was added n-butyflithium (2.5 M/hexanes, 205 mL, 510 mmo)dropwise over a period of 10 minutes. Stirring was maintained at -78 C for I h, andthen a soution of iodine (130 g, 510 mmo) in THF (500 mL) was added dropwise at -78C over a period of 30 minutes. After the addition, the temperature was maintained at -78 C for lh and then aflowed to warm to rt and stirred for a tota? of 18h. The reaction mixture was poured into saturated aqueous Na2SO3 and extracted with EtOAc (2 x 1000 mL). The combined organic extracts were dried over Na2SO4 and concentrated in vacuo to give the tifle compound as an oH (159 g, 96% yied). 1H NMR (500 MHz, CDC3) 67.40 (dd, J= 8.1, 1.4 Hz. IH), 7.32 (t, J= 8.1 Hz, IH). 7.16(dt. J= 8.2, 1.4 Hz, IH).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; RAVULA, Suchitra; SWANSON, Devin M.; SAVALL, Bradley M.; AMERIKS, Michael K.; (250 pag.)WO2016/176449; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 501-29-1, A common heterocyclic compound, 501-29-1, name is 1-Chloro-2-fluoro-4-methoxybenzene, molecular formula is C7H6ClFO, 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.

Reference Example 16; 2-Bromo-4-chloro-5-fluoroaisole (Reference Compound No.16-1) A mixture of 4-chloro-3-fluoroanisole (124 muL, 1.00 mmol) and N-bromosuccinimide was dissolved in mixed solvent of anhydrous N,N-dimethylformamide (0.5 mL) and anhydrous dichloromethane (1 mL), and stirred at 40C for 3 days. After cooling down, chloroform (30 mL) and water (30 mL) were added and partitioned. The water layer was extracted with chloroform (30 mL, 2 times). The combined organic layer was washed with saturated brine (30 mL), dried over anhydrous magnesium sulfate, and then the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to give the titled reference compound (195 mg) as a colorless solid. (Yield 82%)

The synthetic route of 501-29-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Santen Pharmaceutical Co., Ltd; EP1995242; (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. 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, A new synthetic method of this compound is introduced below., Application In Synthesis of 2-Chloro-4-fluorobenzylamine

theta-Oxo-1 -(phenylmethyl^-piperidinecarboxylic acid (0.117 g, 0.5 mmol, prepared as described below) was suspended in dichloromethane (5 ml) and treated with N-(3- dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (0.144 g, 0.75 mmol) and 1-hydroxybenzotriazole (0.102 g, 0.75 mmol). The mixture was stirred at room temperature for 15 minutes and then [(2-chloro-4-fluorophenyl)methyl]amine (0.096 g, 0.6 mmol) was added to the mixture and stirring at room temperature was continued for a further 48 hrs. The mixture was concentrated and partitioned between ethyl acetate and water. The ethyl acetate layer was separated and washed sequentially with 3N aqueous citric acid, water, saturated aqueous sodium hydrogen carbonate, water, and brine and then dried over anhydrous sodium sulphate. Concentration of the organic layer gave an oil which was purified by automated flash silica-gel column chromatography (Biotage SP4), eluting with a gradient of 0-100% ethyl acetate in hexane, to give lambda/-[(2-chloro-4- fluorophenyl)methyl]-6-oxo-1-(phenylmethyl)-2-piperidinecarboxamide (0.1 13 g) as an oil. LC/MS [M+H]+ = 375/377, retention time = 2.63 minutes.

The synthetic route of 15205-11-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2008/116845; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 2533-69-9,Some common heterocyclic compound, 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, molecular formula is C3H4Cl3NO, 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.

To a solution of 4-fluorobenzene-1,2-diamine [Aldrich, 653586] (0.03 g, 0.2 mmol) in acetic acid (1 mL) was added methyl 2,2,2-trichloroethanimidoate [Acros, AC16093-0250] (0.030 mL, 0.24 mmol) dropwise at room temperature. The mixture was stirred at room temperature for 2 h and poured into water (25 mL). The precipitate was separated by filtration and air-dried, which was directly used in the next step without purification.

The synthetic route of 2533-69-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Incyte Corporation; Zou, Ge; Combs, Andrew P.; Buesking, Andrew W.; (62 pag.)US2016/229843; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics