Category: chlorides-buliding-blocks

Synthetic Route of 363-51-9,Some common heterocyclic compound, 363-51-9, name is 2-Chloro-6-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 Schlenk tube was charged with Oxone (0.398 g, 0.648mmol) and trifloroacetic acid (0.099 mL, 1.296 mmol) in anhydrous dioxane (2 mL) under argon. To this mixture was added 2-fluoroaniline (0.06 g, 0.54 mmol), and the reaction mixture was heated to 90 C under argon until starting material was consumed. As the reaction progressed, the color turned from lightred to dark red. The mixture was then cooled to room temperature and washed with a saturated aqueous sodium bicarbonate.The mixture was extracted with EtOAc (2 × 20 mL) and the combined organic layers were dried over Na2SO4. After filtering andremoval of the solvent under reduced pressure in vacuo, theresidue was purified by silica gel (100-200 mesh) column chromatography(hexane-EtOAc, 9:1), to afford a pale-brown solid(65%) of 2-hydroxy-N-trifluoroacetanilides from 2-fluoroaniline(2a).

The synthetic route of 363-51-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Venkateswarlu, Vunnam; Balgotra, Shilpi; Aravinda Kumar; Vishwakarma, Ram A.; Sawant, Sanghapal D.; Synlett; vol. 26; 9; (2015); p. 1258 – 1262;,
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Electric Literature of 870-24-6, 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. 870-24-6, name is 2-Chloroethanamine hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 3: Synthesis of t-butyl (2-chloroethyl)carbamate: 28.7 g (249 mmol) of 2-chloroethylamine hydrochloride was dissolved in 300 ml of dichloromethane. 41 g (192 mmol) of di-t-butyl dicarbonate and 80 ml (576 mmol) of triethylamine were added to the obtained solution, and they were stirred overnight. After the treatmentwith dichloromethane as the extraction solvent in an ordinary manner, the title compound was obtained. Yield: 41 g (229 mmol) (92 %) H-NMR (CDCl3) delta 1.43 (9H, s), 3.41 (2H, dt), 3.59 (2H, t), 4.95 (1H, br)

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-Chloroethanamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Ajinomoto Co., Inc.; EP1065200; (2001); A1;,
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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. 108-41-8, name is 1-Chloro-3-methylbenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: chlorides-buliding-blocks

General procedure: In the test tube were placed 7% Pd/WA30 (19.0 mg, 12.5 mumol), the aryl chloride (250 mumol), the arylboronic acid (375 mumol), Cs2CO3 (163 mg, 500 mumol), and DMA (1 mL). The mixture was stirred at 80 C under an Ar atmosphere. The reaction progress was monitored by TLC analysis (hexane-EtOAc, 5:1). When the reaction was completed within 24 h, the mixture was cooled to r.t., diluted with Et2O (5 mL), and passed through a cotton filter. The catalyst on the filter was washed with Et2O (2 × 15 mL) and H2O (3 × 10 mL). The combined filtrate was separated into two layers. The aqueous layer was extracted with Et2O (20 mL), and the combined organic layers were washed with H2O (4 × 20 mL) and brine (20 mL), dried over Na2SO4, filtered, and concentrated in vacuo. To the residue was added CDCl3 (ca. 1 mL) and 1,4-dioxane (8.53 muL, 100 mumol). After the determination of the reaction yield by 1H NMR, the product was purified by silicagel column chlomatography using hexane-EtOAc (10:1) as eluents to give the corresponding biaryl. When the reaction was incomplete after 24 h, the reaction mixture was treated in the same manner as described above.

The synthetic route of 108-41-8 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Monguchi, Yasunari; Ichikawa, Tomohiro; Netsu, Moeko; Hattori, Tomohiro; Mizusaki, Tomoteru; Sawama, Yoshinari; Sajiki, Hironao; Synlett; vol. 26; 14; (2015); p. 2014 – 2018;,
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These common heterocyclic compound, 2613-32-3, name is 2-Chloro-4,5-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. name: 2-Chloro-4,5-difluoroaniline

1-Chlor-1-dimethylamino-2-methyl-1-propen (64.9 mg, 0.486 mmol) was added to a solution of trans-4-[(pyrazolo[1 ,5-a]pyrim idin-3-ylcarbonyl)am ino]cyclohexanecarboxylic acid (70.0 mg, 0.243 mmol) in dichloromethane (3.1 ml) and the mixture was stirred at roomtemperature for 30 mi Pyridine (59 p1, 0.0.73 mmol) and 2-chloro-4,5-difluoroaniline (39.7 mg, 0.243 mmol, GAS No 261 3-32-3) were added and the mixture was stirred over night at room temperature. For work-up, water was added and the reaction mixture was extracted with dichloromethane. Die organic phase was filtrated through a silicone filter, concentrated and the residue purified by preparative HPLG (Method 9) to yield the title compound (3.8 mg,4% yield).LG-MS (Method 2): R = 1 .10 mm; MS (ESIpos) m/z = 434.1 [M+H].1HNMR (400 MHz, DMSO-d6): 6 [ppm] = 9.62 (5, 1H), 9.32 (dd, 1H), 8.83 (dd, 1H), 8.58 (5,1H), 7.86-7.76 (m, 3H), 7.28 (dd, 1H), 3.90-3.76 (m, 1H), 2.12-1.91 (m, 4H), 1.66-1.50 (m,2H), 1.45-1.31 (m, 2H).

The synthetic route of 2-Chloro-4,5-difluoroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; EIS, Knut; ACKERMANN, Jens; WAGNER, Sarah; BUCHGRABER, Philipp; SUeLZLE, Detlev; HOLTON, Simon; BENDER, Eckhard; LI, Volkhart; LIU, Ningshu; SIEGEL, Franziska; LIENAU, Philip; BAIRLEIN, Michaela; VON NUSSBAUM, Franz; HERBERT,Simon; KOPPITZ, Marcus; (734 pag.)WO2016/177658; (2016); A1;,
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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. 102-49-8, name is 3,4-Dichlorobenzylamine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 102-49-8

General procedure: EDC hydrochloride (1.2 mmol) and HOBt (1.0 mmol) were added at 0 °C to each parallel vial containing a solution of the appropriate acid 44-53 (1 mmol) in dichloromethane, and either cyclohexylamine or 2,3-dichlorobenzylamine (1.5 mmol) was added at the same temperature. After warming up to room temperature, the vials were placed in the Buechi Syncore reactor. Stirring was maintained at 300 rpm overnight and then morpholinomethylpolystyrene (3 equiv/mol) was added. The solutions were kept at room temperature for 1 h, then polymer bound p-toluenesulfonic acid (3 equiv/mol) was added to each vial, and the reaction mixtures were stirred at room temperature for an additional 24 h. The mixtures were filtered and the solutions were evaporated to dryness to give carboxamides 6-25. Solid products were purified by crystallization from ethanol or aqueous ethanol. Oil products were purified by silica gel column chromatography column (dichloromethane as eluent).

According to the analysis of related databases, 102-49-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Piscitelli, Francesco; Ligresti, Alessia; La Regina, Giuseppe; Gatti, Valerio; Brizzi, Antonella; Pasquini, Serena; Allar, Marco; Carai, Mauro Antonio Maria; Novellino, Ettore; Colombo, Giancarlo; Di Marzo, Vincenzo; Corelli, Federico; Silvestri, Romano; European Journal of Medicinal Chemistry; vol. 46; 11; (2011); p. 5641 – 5653;,
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Related Products of 38762-41-3, 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. 38762-41-3, name is 4-Bromo-2-chloroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A 25 mL RBF was subsequently charged with 1.0 mmol aromatic amines, 1.0 mmol 4-hydroxybutan-2-one, 10 mol% I2 (25.4 mg), 2mL DMSO. The resulting mixture was performed at room temperature for 8 h. After reaction was complete, the resulting mixturewas poured into water (20 mL) and extracted with ethyl acetate (3 x10 mL). The combined organic extracts were washed with brine (3 5 mL), then dried over Na2SO4 and concentrated in vacuum. The resulting residue was purified by silica gel columnchromatography (ethyl acetate/petroleum ether 1:20-1:4) to afford the desired products.

The synthetic route of 4-Bromo-2-chloroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Article; Miao, Changqing; Jiang, Liya; Ren, Lanhui; Xue, Qingxia; Yan, Fang; Shi, Weiwei; Li, Xinjian; Sheng, Jiwen; Kai, Shuangshuang; Tetrahedron; vol. 75; 14; (2019); p. 2215 – 2228;,
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Electric Literature of 14862-52-3,Some common heterocyclic compound, 14862-52-3, name is 3,5-Dibromochlorobenzene, molecular formula is C6H3Br2Cl, 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.

3,5-dibromochlorobenzene (2.7 g, 10 mmol), 9-phenylcarbazole-3-boronic acid (6.0 g, 21 mmol), sodium carbonate(10.2 g, 96 mmol), Pd2 (dba) 3 (0.4 g, 0.4 mmol), 50 mL each of toluene, ethanol and water The reaction flask was refluxed under nitrogen for 10 hours and cooled to room temperature. The aqueous layer was washed with ethyl acetate The organic layers were separated and washed with saturated brine and water. The organic layer was dried over magnesium sulfate, filtered, The filtrate was spin dried and passed through a silica gel column to give 4.4 g of product, HPLC purity 99.2%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,5-Dibromochlorobenzene, its application will become more common.

Reference:
Patent; CECEP Wanrun Co., Ltd.; Li Chong; Yu Kaichao; Zhang Zhaochao; (39 pag.)CN107056807; (2017); A;,
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These common heterocyclic compound, 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, 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. Recommanded Product: 4-Bromo-2-chloro-1-fluorobenzene

4-Bromo-2-chloro-l- fluorobenzene (1; 16 g, 76.5 mmol) was dissolved in 50 mL of THF. The reaction mixture was cooled down to -78 C. A solution of LDA in THF (2 M, 38.2 mL, 76.4 mmol) was added dropwise over 20 min. The reaction mixture was stirred at -78 C for 10 min. DMF (8.4 mL) was added dropwise. The reaction mixture was allowed to warm -20 C and quenched with 30 mL of saturated ammonium chloride aqueous solution, extracted with methyl tert- at l ether (50 mL X 3). The combined organic layers were washed with brine, dried over anhydrous Na2S04, and concentrated under reduced pressure to give crude product, which was purified by silica gel chromatography (5-10% EtO Ac/petroleum ether) to afford 8.4 g of 5-bromo-3-chloro-2-fluorobenzaldehyde (2) as white solid (yield: 46%). 1H MR (400 MHz, DMSO-i) delta 10.10 (s, 1H), 8.26 (s, 1H), 7.93 (s, 1H).

The synthetic route of 4-Bromo-2-chloro-1-fluorobenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KARYOPHARM THERAPEUTICS INC.; BALOGLU, Erkan; SENAPEDIS, William; SHACHAM, Sharon; (160 pag.)WO2016/100515; (2016); A1;,
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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. 63624-28-2, name is 2,4-Dimethoxybenzene-1-sulfonyl chloride, A new synthetic method of this compound is introduced below., Formula: C8H9ClO4S

A solution of 2,4-dimethoxybenzene-1-sulfonyl chloride (0.0799 g, 0.337 mmol) and 5-methylbenzo[d]isoxazol-3-amine I60 (0.050 g, 0.34 mmol) in pyridine (1 ml.) was irradiated in the microwave at 110 C for 2 hours. The resultant mixture was loaded onto silica gel and the product purified by column chromatography (12 g S1O2 cartridge, 0-45% EtOAc in petroleum benzine 40-60 C) [205] to yield the title compound (55.0 mg, 42% yield) as a white solid. NMR (400 MHz, CDCb) d 7.86 – 7.82 (m,1H), 7.72 (d, J = 8.81Hz, 1H), 7.37 – 7.28 (m, 2H), 6.49 (d, J = 2.26 Hz, 1H), 6.43 (dd, J = 2.29, 8.82 Hz, 1H), 3.96 (s, 3H), 3.80 (s, 3H), 2.47 (s, 3H). LCMS-A: rt 5.66 min, m/z 348.8 [M+H]+, 347.1 [M-H]

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; CTXT PTY LIMITED; STUPPLE, Paul, Anthony; LAGIAKOS, Helen, Rachel; MORROW, Benjamin, Joseph; FOITZIK, Richard, Charles; HEMLEY, Catherine, Fae; CAMERINO, Michelle, Ang; BOZIKIS, Ylva, Elisabet, Bergman; WALKER, Scott, Raymond; (321 pag.)WO2019/243491; (2019); A1;,
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Some common heterocyclic compound, 61881-19-4, name is 2,2,2-Trifluoro-N-phenylacetimidoyl chloride, molecular formula is C8H5ClF3N, 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. Product Details of 61881-19-4

General procedure: A mixture of acetimidoyl chloride (1 mmol), sodium azide (1 mmol), and acetonitrile (3 mL) was irradiated in a microwave oven at 300 W for 8-10 min, after completion of the reaction, as indicated by TLC, the reaction mixture was filtered. After removing the solvent under reduced pressure, if necessary, the crude products were purified by washing with n-hexane to give the target product 3a-3j (90-95%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 61881-19-4, its application will become more common.

Reference:
Article; Rahmani, Fariba; Darehkordi, Ali; Notash, Behrouz; Journal of Fluorine Chemistry; vol. 166; (2014); p. 84 – 87;,
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