Tag: M.W=300-400

Reference of 13985-15-4, 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. 13985-15-4 name is 2,3,6,7-Tetramethoxy-9,10-dimethylanthracene, 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.

General procedure: To a gently refluxing solution of the anthracene (1a-1c) (1mmol) in 1,2-dichloroethane (50mL) was added portionwise 5-nitrobenzenediazonium-2-carboxylate (2.5mmol). When TLC showed that the starting anthracene was consumed, the reaction mixture was concentrated under reduce pressure. The residue was purified by flash column chromatography on silica gel with petroleum ether: CH2Cl2=4:1 (v/v) as eluent to yield the triptycene as a pale yellow solid. 2b: 67mg, 15% yield. 1H NMR (300MHz, CDCl3): delta 8.08 (s, 1H), 7.87 (d, 1H, J=6.9Hz), 7.37 (d, 1H, J=8.2Hz), 6.98 (s, 2H), 6.97 (s, 2H), 3.86 (s, 12H), 2.46 (s, 3H), 2.43 (s, 3H). 13C NMR (75MHz, CDCl3): delta 156.4, 151.2, 146.3, 146.2, 145.1, 140.4, 139.9, 120.9, 120.4, 115.0, 106.2, 106.0, 56.42, 56.38, 48.5, 48.3, 13.9, 13.7. EI-TOF-MS: m/z 447 [M]+. Anal. calcd. for C26H25NO6·0.1CH2Cl2: C, 68.75; H, 5.57; N, 3.07. Found: C, 68.81; H, 5.80; N, 2.97.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,3,6,7-Tetramethoxy-9,10-dimethylanthracene, and friends who are interested can also refer to it.

Reference:
Article; Li, Peng-Fei; Han, Ying; Chen, Chuan-Feng; Chinese Chemical Letters; vol. 26; 7; (2015); p. 839 – 842;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 57602-02-5, name is 1,14-Dibromo-3,6,9,12-tetraoxatetradecane, belongs to ethers-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 57602-02-5, category: ethers-buliding-blocks

1,14-dibramo-3,6,9,12-tetraoxatetradecane (3.35 g, 9.2 mmol) and sodium methanethiosulfonate (2.48 g, 18.5 mmol) were dissolved in dry DMF (40 mL) and stirred at room temperature for 3 days. The solvent was evaporated. The residue was purified by column chromatography on SiO2. Elution with ethyl acetate/hexane (9:1) afforded, after evaporation, 1-(14-bromo-3,6,9,12-tetraoxatetradecyl) methanethiosulfonate (0.85 g) as a pale yellow oil and tetraoxatetradecane-1,14-diyl-bis-methanethiosulfonate (useful as a cross linker) as a slightly yellow colored oil (1.64 g).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1,14-Dibromo-3,6,9,12-tetraoxatetradecane, and friends who are interested can also refer to it.

Reference:
Patent; Dime, David S.; Backx, Peter; Kimmeldirk, Klaus; EP966304; (2005); B1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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 88149-49-9 as follows. Formula: C7H4Br2F3NO

a) N-(2,6-dibromo-4-(trifluoromethoxy)phenyl)acetamide To a solution of 2,6-dibromo-4-(trifluoromethoxy)aniline (5.0 g, 14.9 mmol) in acetic acid (10 mL) was added acetic anhydride (2.1 mL, 22.5 mmol) and the mixture stirred for 48 hrs at 90° C. The resulting residue was cooled to room temperature, poured into ice water and the resulting precipitate collected by filtration, washed with water and dried under vacuum to yield N-(2,6-dibromo-4-(trifluoromethoxy)phenyl)acetamide.

According to the analysis of related databases, 88149-49-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Janssen Pharmaceutica NV; Sui, Zhihua; Subasinghe, Nalin; US2014/275172; (2014); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 57602-02-5, name is 1,14-Dibromo-3,6,9,12-tetraoxatetradecane, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 57602-02-5

Example 2 Synthesis of Double End-Substituted Pentaethyleneglycol-Sumatriptan (SMQT-02) Sumatriptan (236 mg, 0.8 mmol) is dissolved in 2 mL dry DMF, 60% NaH (32 mg, 0.8 mmol) is added, stirred and react 15 minutes, triethylene glycol 2-bromoethyl (145.6 mg, 0.4 mmol) is added, and reaction is performed overnight under nitrogen gas protection. Water is added to the above reaction liquid to quench the reaction, extraction is performed three times by using acetic ether, an organic phase is dried by using anhydrous sodium sulfate, concentrate goes through column separation to obtain 184 mg product, with a yield rate 58%. 1H-NMR (CDCl3): 2.34 (s, 12H), 2.70 (t, 4H), 2.72 (s, 6H), 2.94 (t, 4H), 3.06 (t, 4H), 3.40 (t, 4H), 3.49 (s, 12H), 4.35 (s, 4H), 6.98 (s, 2H), 7.11 (d, 2H), 7.23 (d, 2H), 7.60 (s, 2H), 8.91 (s, 2H).

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 57602-02-5.

Reference:
Patent; JENKEM TECHNOLOGY CO.,LTD.(TIANJIN); XU, Lihua; ZHAO, Xuan; FENG, Zewang; WANG, Jinliang; WANG, Zhenguo; (16 pag.)US2016/82117; (2016); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 13985-15-4, These common heterocyclic compound, 13985-15-4, name is 2,3,6,7-Tetramethoxy-9,10-dimethylanthracene, 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.

FIG. 17 shows schematically the methods by which the substituted precursor compounds were prepared. The tested products are labelled CMR 1 (R1-R4=-OCH3); CMR 4 (R1-R4=-CO2CH3); and CMR 6 (R1-R4?N-substituted cyclic imido).

Statistics shows that 2,3,6,7-Tetramethoxy-9,10-dimethylanthracene is playing an increasingly important role. we look forward to future research findings about 13985-15-4.

Reference:
Patent; Ke, Chenfeng; Davis, Anthony P.; US2015/147275; (2015); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 88149-49-9, 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. 88149-49-9, name is 2,6-Dibromo-4-(trifluoromethoxy)aniline belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The acid chloride reaction is completed, and 90.5 g (0.27 mol) of 2,6-dibromo-4-trifluoromethoxyaniline is added to the reaction vessel. Add catalyst 2 g of zinc chloride (0.015 mol) and benzoyl peroxide 2.5g (0.01mol), Rinse at 90 ° C for 4 h, The amidation incubation reaction is carried out. (3) Post-treatment: After the amidation reaction was completed, 80 mL of toluene was removed under reduced pressure, 100 mL of water was added, and 20 mL of toluene was removed under reduced pressure, and the temperature was lowered to 40 ° C. Filtration to obtain 124.9 g of solid thiazolamide. The purity was 96.7percent, and the yield was 91.5percent.

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, 2,6-Dibromo-4-(trifluoromethoxy)aniline, other downstream synthetic routes, hurry up and to see.

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. 88149-49-9, name is 2,6-Dibromo-4-(trifluoromethoxy)aniline, A new synthetic method of this compound is introduced below., Recommanded Product: 88149-49-9

Step one: 0.237 mol,52.63 g of 2-methyl-4-trifluoromethyl-5-thiazolecarboxylic acid(content 95percent)With 0.261 mol,89.2 g of 2,6-dibromo-4-trifluoromethoxyaniline (content 98percent)As for a certain amount of acetonitrile,Warm up to 55°C,Stir for about 0.5 h;Step two:A 0.261 mol catalyst was slowly added dropwise to the above reactants.40 g phosphorus oxychloride,After the addition,Warming to reflux,Insulation reflux reaction,The control was almost complete,The reaction time is about 8 h;Step 3:The above product is lowered to room temperature,Slowly drip it into a certain amount of crushed ice.Then stir for 0.5 h,The target product thiadiamide is obtained.Filter and dry, weigh:112.2 g detected purity: 94.3percent, yield: 84.6percent.

The synthetic route of 88149-49-9 has been constantly updated, and we look forward to future research findings.

Application of 13985-15-4, 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. 13985-15-4 name is 2,3,6,7-Tetramethoxy-9,10-dimethylanthracene, 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.

FIG. 17 shows schematically the methods by which the substituted precursor compounds were prepared. The tested products are labelled CMR 1 (R1-R4=-OCH3); CMR 4 (R1-R4=-CO2CH3); and CMR 6 (R1-R4?N-substituted cyclic imido).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,3,6,7-Tetramethoxy-9,10-dimethylanthracene, and friends who are interested can also refer to it.

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. 1840-97-7, name is 2,4-Dibromo-1-(trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., Product Details of 1840-97-7

Add 1008 g of 2,4-dibromotrifluoromethoxybenzene, 5200 mL of DMF to the reaction vessel, and control the temperature to 150 C.Slowly add 774 g of cuprous cyanide solids with stirring.During the addition, the temperature should not exceed 155 C. After the addition, the reaction is stirred and the GC is traced until the reaction is over.After the reaction is completed, it is cooled, and the reaction product is poured into water to analyzeSolid, suction filtration,Extraction with 1,2-dichloroethane, followed by suction filtration, liquid separation, rotary evaporation, drying,Obtained a white powdery solid2,4-dicyanotrifluoromethoxybenzene 326 g,The yield was 49%.

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.

Electric Literature of 2062-98-8, These common heterocyclic compound, 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, 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.

Example 11 A mixture of ethanolamine (13 g, 28 mmole) and ether (30 mL) was cooled to 15 C. Perfluoro-2-methyl-3-oxahexanoyl fluoride (33 g in ether 50 mL) was added dropwise to keep the reaction temperature below 25 C. After the addition, the reaction mixture was stirred at room temperature for one hour. The solid was removed by filtration and the filtrate was washed with hydrochloric acid (0.5N, 30 mL), water (2 times 30 mL), sodium hydrogen carbonate solution (0.5N, 20 mL), water (30 mL), and sodium chloride solution (saturated, 20 mL). It was then concentrated and dried in vacuum over night at room temperature to give a white solid 35 g, yield 95%. H NMR (CDCl3) 1.67 (br s, 1H), 3.57 (m, 2H), 3.80 (t, J=5 Hz, 2H), 6.91 (br s, 1H) ppm. F NMR (CDCl3) -81.2 (dm, J=148 Hz, 1F), -81.7 (t, J=7 Hz, 3F), -82.7 (d, J=3 Hz, 3F), -85.2 (dm, J=148 Hz, 1F), -130.1 (s, 2F), -133.2 (m, 1F) ppm. The product is N-(perfluoro-2-methyl-3-oxahexanoyl)-2-aminoethanol. A 250-mL flask was charged with triethylamine (8.2 g), THF (80 mL), and N-(perfluoro-2-methyl-3-oxo-hexanoyl)-2-aminoethanol (25 g). Methacryloyl chloride (8.44 g in tetrahydrofuran, 20 mL) was added dropwise to the above mixture at 5 C. The mixture was stirred at room temperature overnight. The reaction mixture was poured into water (200 mL) and two layers were formed. The aqueous layer (top layer) was extracted with methylene chloride (five time 50 mL). The combined methylene chloride extracts and original organic layer were washed with water (six times 60 mL), neutralized with dilute hydrochloric acid (0.5N), dried over anhydrous sodium sulfate, concentrated and dried on vacuum to give a oil, N-(perfluoro-2-methyl-3-oxahexanoyl)-2-aminoethyl methacrylate (27.06 g), yield 92%. H NMR (CDCl3) 1.94 (m, 3H), 3.72 (m, 2H), 4.33 (m, 2H), 5.63 (m, 1H), 6.12 (m, 1H), 6.88 (br s, 1H) ppm. F NMR (CDCl3) -81.2 (dm, J=148 Hz, 1F), -81.7 (t, J=7 Hz, 3F), -82.7 (d, J=3 Hz, 3F), -85.2 (dm, J=148 Hz, 1F), -130.1 (s, 2F), -133.4 (m, 1F) ppm.

Statistics shows that Perfluoro(2-methyl-3-oxahexanoyl) fluoride is playing an increasingly important role. we look forward to future research findings about 2062-98-8.