Tag: M.W=100-200

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. 821-10-3, name is 1,4-Dichlorobut-2-yne belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C4H4Cl2

General procedure: A solution of 1,4-dichloro-2-butyne (1.23 g, 10 mmol) and the respective N-alkylazole (20 mmol) in MeCN (15 mL) was stirred at 80 C for 24 h. The precipitate wascollected by filtration, washed with MeCN, and dried under reduced pressure.

The synthetic route of 821-10-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Haslinger, Simone; Laus, Gerhard; Oberparleiter, Stefan; Wurst, Klaus; Kahlenberg, Volker; Nerdinger, Sven; Schreiner, Erwin; Schottenberger, Herwig; Heterocycles; vol. 95; 2; (2017); p. 1148 – 1158;,
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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 1435-48-9 as follows. Product Details of 1435-48-9

Into a four necked RB flask of 1-lit capacity equipped with over head stirrer, a glass condenser and addition funnel, DCFB (250 g, 1.51 mol) and A1C13 (322 g, 2.41 mol) were added. The suspension was stirred at room temperature. Acetyl chloride (125 g, 1.60 mol) was added drop wise within two hours by maintaining the temperature 30-350C. After complete addition of acetyl chloride the mixture was quickly heated to 110-1200C for 5-6 hrs. The reaction kinetics was monitored by taking samples every two hrs. After the reaction was stopped the crude reaction mixture was cooled to ambient temperature. Then the reaction mixture was quenched using 1 kg ice and 500 ml water maintaining the temperature below 5O0C. The aqueous layer thus obtained was extracted with 200 ml of DCM thrice and combined all the extracts for evaporation. After the evaporation of DCM, 298.8g of brown product was obtained with the following composition.% Conversion of DCFB by GC = 76 % (24% DCFB as solvent)% DCFA = 68.64 %% Selectivity by GC = 91.5 %% Isomer = 4-5 %% DCFB = 24 %% H. B. = 4.1 %

According to the analysis of related databases, 1435-48-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ADITYA BIRLA SCIENCE & TECHNOLOGY CO. LTD.; MANDAL, Sisir; PATIL, Narendra; SULEMAN, Inamdur; MORE, Vinod; PURI, Prashant; WO2010/58421; (2010); A2;,
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Synthetic Route of 108-70-3, 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 108-70-3 as follows.

1-Bromopropane (25 g, 0.20 mol) was added dropwise to a mixture of Mg (5.0 g, 0.21 mol) in diethyl ether (100 mL) at room temperature. The mixture was refluxed for 2 h and then cooled to room temperature. The new prepared Grignard reagent was then added to a mixture of 1,3,5-trichlorobenzene (10.4 g, 570 mmol) and Ni(dppe)Cl2 (75 mg, 0.14 mmol) in 100 mL of diethyl ether at room temperature. The mixture was stirred overnight and quenched by adding a saturated aqueous NH4Cl. The resulting mixture was extracted with ether, and washed with deionized water. The organic layer was separated and dried over Na2SO4. The solvent was removed under reduced pressure and the residue was purified by flash chromatography to give 1,3,5-trialkylbenzene (9.75 g, 84%) as a colorless oil.

According to the analysis of related databases, 108-70-3, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Taoping; Zhao, Xiaoming; Shen, Qilong; Lu, Long; Tetrahedron; vol. 68; 32; (2012); p. 6535 – 6547;,
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Synthetic Route of 39065-95-7, 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. 39065-95-7, name is 4-(Chlorodifluoromethoxy)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a reaction flask were added 6-chloro-5-bromonicotinic acid (1.17 g, 4.97 mmol), 4-(chlorodifluoromethoxy)aniline (0.8 g, 4.15 mmol), dissolved with 20 mL anhydrous DMF, 2-(7-aza-1H-benzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate (HATU, 2.1 g, 5.39 mmol) and N,N-diisopropylethylamine (DIPEA, 534 mg, 4.15 mmol) were added, and the reaction was stirred under nitrogen protection at room temperature for 18 hours. The reaction was diluted with large amount of water, extracted with ethyl acetate for 3-4 times, the organic layers were combined, washed with brine, concentrated, purified by column chromatography, dried in vacuum to afford 1.18 g of a product, yield: 69.5%.

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-(Chlorodifluoromethoxy)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shenzhen Targetrx, Inc.; WANG, Yihan; ZHAO, Jiuyang; AL, Yixin; (55 pag.)EP3553056; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 2106-04-9,Some common heterocyclic compound, 2106-04-9, name is 3-Chloro-2-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: A mixture of substituted aniline (0.8 mmol), potassiumcarbonate (553 mg, 4 mmol), and potassium iodide(13 mg, 0.08 mmol) in acetone (12 ml) was sitrred at roomtemperature. To the suspension, a solution of compound9 (179 mg, 0.8 mmol) was added in acetone (6 ml) dropwise.The reaction was stirred for 8 h and monitored byTLC. Solvent was removed under vaccum, followed bythe addition of ethyl acetate (40 ml) and water (30 ml).The organic layer was washed with water (30 ml × 1) andbrine (30 ml × 1), dried with anhydrous sodium sulfate,filtered, and concentrated. The crude material wasabsorbed onto silica gel and purified using 90% of petroleumether in ethyl acetate to yield title compound 10.

The synthetic route of 2106-04-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Guo, Guangzhu; Liu, Jianzhen; Wang, Guanjie; Zhang, Daoguang; Lu, Jinjie; Zhao, Guisen; Anti-Cancer Drugs; vol. 27; 4; (2016); p. 278 – 285;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 6781-98-2, name is 2-Chloro-1,3-dimethylbenzene, 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 6781-98-2, Quality Control of 2-Chloro-1,3-dimethylbenzene

General procedure: To a 50 mL Schlenk tube containing base (1.5 mmol) and precatalyst 4a (1 mol percent, 0.0083 g) purged with N2 (three times), amine (1.2 mmol) was added via syringe, and the resulted mixture was allowed to stir at room temperature for 2?3 min. Solvent (1 mL) was then injected via syringe followed by the aryl chloride (1.0 mmol). If the aryl chloride was a solid, it was introduced into the vial prior to purging with N2. At this time, the reaction was stirred for 24 h at 100 °C. After cooling to the room temperature, the reaction mixture was concentrated in vacuo and directly purified via silica gel flash chromatography. 2,6-Dimethyl-N-phenylaniline (16) ;1H NMR (CDCl3, 400 MHz, 298 K): delta=7.14-7.07 (m, 5H), 6.71 (t, J=6.8 Hz, 1H), 6.47 (d, J=7.6 Hz, 2H), 5.09 (br s, 1H), 2.18 (s, 6H); 13C NMR (CDCl3, 100 MHz, 298 K): delta=146.19, 138.14, 135.84, 129.16, 128.47, 125.68, 118.08, 113.41, 18.28.

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:
Article; Fang, Weiwei; Jiang, Jian; Xu, Yong; Zhou, Juefei; Tu, Tao; Tetrahedron; vol. 69; 2; (2013); p. 673 – 679;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 10061-02-6, name is trans-1,3-Dichloropropene, molecular formula is C3H4Cl2, 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 trans-1,3-Dichloropropene

Example 3 (E)-2-(1-Methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methyl-6-(3-chloroprop-2-enyloxy)pyridine A mixture of 6-hydroxy-2-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methylpyridine (0.9 g, 3.3 mmol) and NaH (60 % in oil, 0.16 g, 4 mmol) in acetonitrile (20 ml) and DMF (1 ml) is stirred for 10 min at ambient temperature and (E)-1,3-dichloropropene (0.4 g, 3.6 mmol) is added. After stirring for 60 h at ambient temperature, the remaining NaH is deactivated and the resulting mixture is diluted with pentane/ethyl acetate (by volume ration 1/1) and filtered through a bed of silica gel. The filtrate is washed with water. The organic layer is dried with anhydrous magnesium sulfate, filtered and evaporated in vacuo. Purification by flash chromatography (silica gel: pentane/ethyl acetate 9/1 v/v) yields the title compound (0.6 g, 52 % yield) as an colorless oil.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 10061-02-6, its application will become more common.

Reference:
Patent; American Cyanamid Company; EP955300; (1999); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1871-57-4,Some common heterocyclic compound, 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene, molecular formula is C4H6Cl2, 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.

1.0kg 3-chloro-2-chloromethylprop-1-ene,37.6g pinacol and 28.6g dibenzo-18-crown-6 were dissolved in 4.2kg tribromomethane,At a temperature controlled at 18-25 degrees, dropwise add 3.2kg of sodium hydroxide and 460g of potassium bromide to dissolve in 3.2kg of aqueous solution.Reaction for 50 hours; after the reaction is complete, add water and toluene, filter through celite pad,Wash the filter cake, combine the filtrates, separate the liquid, collect the organic phase, and concentrate to a small volume,Add n-heptane to crystallize at 0 degree, filter,Drying gave 1.185kg 1,1-dibromo-2,2-bis(chloromethyl)cyclopropane, light yellow solid, yield 50%, HPLC purity 98.7%.

The synthetic route of 1871-57-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Aisite (Chengdu) Bio-pharmaceutical Co., Ltd.; Wang Yin; Ha Leikeruishennan·kelatuer·nalaximuhan·kunqitapadamu; La Gehaiwende·laao·moshala; Zhao Zhenyu; Xu Hui; Guo Peng; (9 pag.)CN110759840; (2020); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 433-94-3, 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. 433-94-3 name is 2-Chloro-6-(trifluoromethyl)aniline, 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.

Step A: 4-bromo-2-chloro-6-(trifluoromethyl)aniline N-bromo succinimide (910 mg, 5.1 mmol) was added to a solution of 2-chloro-6-(trifluoromethyl)aniline (1.0 g, 5.1 mmol) and acetic acid (3 mL) in acetonitrile (10 mL) at room temperature. The mixture was heated at reflux, with stirring, for 18 h. The reaction mixture was then filtered through Celite and concentrated to give the title compound, which was used in the next step without further purification.

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

Reference:
Patent; Valeant Pharmaceuticals North America; US2008/139610; (2008); 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. 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine

Weigh the intermediate 1-e (50 mg, 0.27 mmol)1-methyl-1H-pyrazole-4-boronic acid pinacol ester (55 mg, 0.27 mmol)2N aqueous Na2CO3 solution (0.27 ml, 0.54 mmol)Bis (triphenylphosphine) palladium (II) chloride (19 mg, 0.027 mmol)Dioxane (5 ml) was added to the flask and heated to 70 C for 16 h.After stopping the reaction,To the reaction solution was added 100 ml of water,Stir,Ethyl acetate (20 ml * 4)Drying the ester layer with anhydrous sodium sulfate,Concentrated, separated by column chromatography (petroleum ether: ethyl acetate = 5: 1),A yellow solid (55 mg, 88%) was obtained.

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 918538-05-3.

Reference:
Patent; Jiangsu Xiansheng Pharmaceutical Co., Ltd.; Xin Minxing; Wen Jun; Tu Chongxing; Liu Zhaoyu; Shen Han; Wang Mengyu; Zhao Xinge; (36 pag.)CN104003990; (2017); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics