Tag: M.W=200-300

Electric Literature of 13918-92-8, 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 13918-92-8 as follows.

To an ice cooled solution of 5′-amino-7′-nitrospiro[cyclobutane-1,3′-indolin]-2′- one (2.0 g, 8.58 mmol) in DCM (20 mL) were added pyridine (1.4 mL, 17.16 mmol) followed by 2,4-difluorobenzenesulfonyl chloride (1.7 mL, 12.87 mmol) dropwise. The mixture was at RT for 3 h. The mixture was diluted with DCM (100 mL), washed with water (100 mL) and brine (100 mL), dried over sodium sulphate and concentrated under reduced pressure to afford the title compound as yellow solid (2.5 g, 89 %.).1H NMR (400 MHz, DMSO-d6): delta 11.0 (s, 1H), 10.86 (s, 1H), 7.95-7.83 (m, 1H), 7.68 (d, J=1.5 Hz, 1H), 7.62 (d, J=1.5 Hz, 1H), 7.56 (t, J=8.8 Hz, 1H), 7.30-7.25 (m, 1H), 2.47-2.40 (m, 2H), 2.35-2.12 (m, 4H).

According to the analysis of related databases, 13918-92-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ORION CORPORATION; UJJINAMATADA, Ravi Kotrabasaiah; SAMAJDAR, Susanta; ABBINENI, Chandrasekhar; MUKHERJEE, Subhendu; LINNANEN, Tero; WOHLFAHRT, Gerd; (220 pag.)WO2016/203112; (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. 33863-76-2, name is 1-Bromo-3-chloro-5-fluorobenzene, A new synthetic method of this compound is introduced below., Safety of 1-Bromo-3-chloro-5-fluorobenzene

A mixture of 1-bromo-3-chloro-5-fluorobenzene (8Og, 480mmol), zinc cyanide (33.65g, 290mmol) and zinc dust (0.94g, 14.46mmol) in DMF (34OmL) was stirred at rt for 5 min. Dichloro[1 ,1 ‘- EPO bis(diphenylphosphino)ferrocene] palladium(ll) (4.99g, 16mmol) was then added and the mixture was heated under reflux for 50 min. The reaction mixture was cooled to rt and filtered through Arbocel, washing through with diethyl etherpentane (50:50, 7 x 10OmL). The phases were separated and the organic phase was diluted with water (10OmL) and extracted with further diethyl ethe?pentane (50:50, 3 x 10OmL). The combined organic solutions were then washed with water, dried over magnesium sulfate and concentrated in vacuo. Distillation of the residue under reduced pressure afforded the title compound as a colourless solid in 66% yield, 48.5g. LRMS: m/z APCI 155 [MH+]

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; PFIZER LIMITED; WO2006/67587; (2006); A2;,
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Application of 1096296-85-3, A common heterocyclic compound, 1096296-85-3, name is (5-Bromo-2-chlorophenyl)methanamine, molecular formula is C7H7BrClN, 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.

To a solution of (5-bromo-2-chloro-phenyl)methanamine (6.5 g, 29.7 mmol) and triethylamine (TEA) (6 g, 59.4 mmol) in CH2CI2 was added methyl chloroformiate (3.35 g, 35.6 mmol) dropwise at 0 C. Then the reaction mixture was stirred at 25C for 10 hours. The reaction mixture was concentrated, diluted with EtOAc(300 mL), washed with brine, and dried over Na2S04. Concentration under reduced pressure gave methyl N-[(5-bromo-2-chloro- phenyl)methyl]carbamate (4 g, yield 49%).

The synthetic route of 1096296-85-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF SE; WINTER, Christian; RHEINHEIMER, Joachim; WOLF, Antje; TERTERYAN, Violeta; POONOTH, Manojkumar; WIEBE, Christine; KREMZOW-GRAW, Doris; ROeHL, Franz; ROHRER, Sebastian Georgios; WIEJA, Andy; ROSENBAUM, Claudia; GRAMMENOS, Wassilios; WO2014/202703; (2014); A1;,
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Reference of 110407-59-5, 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. 110407-59-5, name is 2-Chloro-4-fluorobromobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 1; Synthesis of (+)-4-chloro-2-fluoro-9-trifluoromethyl-9H-fluoren-9-ol (compound No. 526); Step 1; 2′-chloro-4′-fluoro-biphenyl-2-carboxylic acid ethyl ester; To a reaction vessel were added 1-bromo-2-chloro-4-fluorobenzene (25 g), ethyl 2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzoate (46 g), toluene (125 ml), water (125 ml) and tripotassium phosphate (50.5 g), and purged with argon. To this mixture was added dichlorobis(triphenylphosphine)palladium(II) (1.67 g) and the mixture was stirred in an oil bath at 110 C. for 3 hr. The oil bath was removed, and water (125 ml) was added to the reaction mixture. The mixture was stirred at room temperature for 1 hr, and filtered through celite. The filtrate was partitioned in a separatory funnel. The aqueous layer was extracted with toluene, and the organic layers were combined. The organic layer was washed twice with water (125 ml), dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to give the title compound (41.8 g). The obtained solid was directly used for the next reaction without further purification.1H-NMR (CDCl3) delta: 8.06-8.02 (1H, m), 7.60-7.54 (1H, m), 7.52-7.45 (1H, m), 7.27-7.16 (3H, m), 7.06-7.00 (1H, m), 4.18-4.09 (2H, m), 1.11-1.06 (3H, m).

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-Chloro-4-fluorobromobenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; JAPAN TOBACCO INC.; US2010/240634; (2010); 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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 19752-55-7

General procedure: To a flask containing dried LiCl (0.35 g, 8.24 mmol) was added iPrMgCl (2 M in THF, 4.1 mL) and THF (5 mL) at 15¡ã C. After beingstirred for 15 min, 3-bromo-1-benzonitrile (1.46 g, 8.03 mmol) inTHF (1 mL) was added to the reaction mixture and the obtainedmixture was stirred for 15 min. Then, DMF (1.3 mL, 12 mmol) wasadded at 0¡ã C and the mixture was stirred for 2 h. Then, aq NH3 (7 mL, 28-30percent) and I2 (4.06 g, 16 mmol) were added to the reaction mixture. After being stirred for 2 h at room temperature, the reactionmixture was poured into satd aq Na2SO3 solution and was extracted with CHCl3 (3?30 mL). The organic layer was dried over Na2SO4 and filtered. After removal of the solvent, the residue waspurified by short column chromatography on silica gel (eluent:hexane/ethyl acetate=9:1, v/v) to provide pure 1,3-dicyanobenzene (0.73 g) in 71percent yield. Most nitriles mentioned in this work are commercially availableand were identified by comparison with the authentic samples.

According to the analysis of related databases, 19752-55-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Ishii, Genki; Harigae, Ryo; Moriyama, Katsuhiko; Togo, Hideo; Tetrahedron; vol. 69; 5; (2013); p. 1462 – 1469;,
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Adding a certain compound to certain chemical reactions, such as: 89794-02-5, name is 4-Bromo-2-chlorotoluene, 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 89794-02-5, Product Details of 89794-02-5

Example P14: Preparation of 2-(4-bromo-2-chlorophenyl)-1-methyl-ethylamine (compound no. Z1.451): a) Preparation of 4-bromo-2-chloro-1-dibromomethyl-benzeneA mixture of 4-bromo-2-chlorotoluene (10 g, 48.6 mmol), N-bromosuccinimide (43.3 g, 243.3 mmol), benzoyl peroxide (0.5 g) and CCI4 (80 ml) was heated to reflux for 6 h. Completion of the reaction was confirmed by TLC. After cooling a yellow precipitate was isolated by filtration and washed with CCI4. The organic layer was concentrated and both the concentreated organic layer and the precipitate were purified by chromatography using silica column (60-120 mu mesh) and hexane as eluent. 17.5 g (98% of theory) of 4-bromo-2-chloro- 1-dibromomethyl-benzene was obtained. 1HNMR (400 MHz, CDCI3):- 7.02 delta (s, 1 H), 7.5 delta (dd, 2H), 7.87 delta (d,1H,CHBr2),

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; SYNGENTA PARTICIPATIONS AG; SYNGENTA LIMITED; WO2007/141009; (2007); A1;,
Chloride – Wikipedia,
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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. 5719-08-4, name is 4-Chloro-9H-pyrimido[4,5-b]indole belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C10H6ClN3

3.9. 4,6-Dichloro-9-(2,3,5-tri-O-benzoyl-b-D-ribofuranosyl)-pyrimido[4,5-b]indole (13) : Pyrimidoindole 11 (200 mg, 0.84 mmol) was suspended in acetonitrile (5 ml) and BSA (206 ll, 0.84 mmol) was added. Reaction mixture was stirred for 10 min at rt., TMSOTf (308 ll, 1.68 mmol) and protected ribofuranose (430 mg, 0.84 mmol) were added. Mixture was heated to 60 C for 8 h. After cooling to rt, the mixture was extracted with EtOAc and water, organic layer was washed with NaHCO3 and again with water, dried over MgSO4 and evaporated under reduced pressure. Crude product was purified using column chromatography (hexane/EtOAc, 0-40% EtOAc). After crystallization from chloroform/methanol mixture, nucleoside 13 (572 mg, 54%) was observed as white crystals; 3.10 4-Chloro-9-(2,3,5-tri-O-benzoyl-beta-d-ribofuranosyl)-pyrimido[4,5-b]indole (14) : Compound 14 was prepared as described for 13 from pyrimidoindole 12 (300 mg, 1.5 mmol) to give 440 mg (46%) of white crystals; mp 178-182 C, IR (ATR): nu = 2360, 2336, 1718, 1546, 1442, 1261, 1090, 1068, 704 cm-1. H NMR (600.1 MHz, DMSO-d6): 4.69 (dd, 1H, Jgem = 12.4, J5’b,4′ = 4.2, H-5’b); 4.85 (dd, 1H, Jgem = 12.4, J5’a,4′ = 3.2, H-5’a); 4.91 (ddd, 1H, J4′,3′ = 6.6, J4′,5′ = 4.2, 3.2, H-4′); 6.36 (t, 1H, J3′,2′ = J3′,4′ = 6.6, H-3′); 6.61 (dd, 1H, J2′,3′ = 6.6, J2′,1′ = 4.6, H-2′); 7.03 (d, 1H, J1′,2′ = 4.6, H-1′); 7.41 (m, 2H, H-m-Bz-2′); 7.50 (m, 4H, H-m-Bz-3′,5′); 7.51 (ddd, 1H, J6,5 = 7.8, J6,7 = 7.3, J6,8 = 1.0, H-6); 7.57 (ddd, 1H, J7,8 = 8.4, J7,6 = 7.3, J7,5 = 1.3, H-7); 7.62 (m, 1H, H-p-Bz-2′); 7.68 (m, 2H, H-p-Bz-3′,5′); 7.84 (m, 2H, H-o-Bz-2′); 7.93 (m, 2H, H-o-Bz-5′); 7.99 (m, 2H, H-o-Bz-3′); 8.10 (ddd, 1H, J8,7 = 8.4, J8,6 = 1.0, J8,5 = 0.7, H-8); 8.35 (ddd, 1H, J5,6 = 7.8, J5,7 = 1.3, J5,8 = 0.7, H-5); 8.78 (s, 1H, H-2). 13C NMR (150.9 MHz, DMSO-d6): 63.1 (CH2-5′); 70.3 (CH-3′); 72.2 (CH-2′); 78.8 (CH-4′); 86.2 (CH-1′); 112.1 (CH-8); 112.4 (C-4a); 118.0 (C-4b); 122.9 (CH-5); 123.3 (CH-6); 128.6, 128.8 (C-i-Bz); 128.9 (CH-m-Bz); 129.0 (CH-7); 129.3 (CH-o-Bz-5′); 129.4 (C-i-Bz); 129.5 (CH-o-Bz-2′); 129.6 (CH-o-Bz-3′); 133.8, 134.1 (CH-p-Bz); 138.4 (C-8a); 152.1 (C-4); 154.0 (C-2-furyl); 154.0 (CH-2); 155.3 (C-9a); 164.8 (COPh-2′); 165.0 (COPh-3′); 165.5 (COPh-5′). ESI MS m/z (rel.%): 670 (100) [M+Na], 672 (33) [M+2+Na]. HR MS (ESI) for C36H27ClN3O7 [M+H]: calcd 648.15320; found 648.15318.

The synthetic route of 5719-08-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Tichy, Michal; Pohl, Radek; Hocek, Michal; Xu, Hao Ying; Chen, Yen-Liang; Yokokawa, Fumiaki; Shi, Pei-Yong; Bioorganic and medicinal chemistry; vol. 20; 20; (2012); p. 6123 – 6133,11;,
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Adding a certain compound to certain chemical reactions, such as: 50594-82-6, name is 3,4,5-Trichlorobenzotrifluoride, 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 50594-82-6, HPLC of Formula: C7H2Cl3F3

EXAMPLE (II-1) STR36 12.5 g (0.05 mol) of 3,4,5-trichloro-benzotrifluoride are added slowly to a stirred mixture, heated to 60 C., of 8.0 g (0.05 mol) of 2,7-dihydroxy-naphthalene, 4.2 g (0.075 mol) of potassium hydroxide powder and 100 ml of dimethyl sulphoxide, and stirring of the reaction mixture is continued for approximately 3 hours at 60 C. After the mixture has cooled to approximately 20 C., it is diluted with water and methylene chloride and filtered. The organic phase is separated from the filtrate, washed with water, dried using sodium sulphate and filtered. The solvent is distilled off from the filtrate under a waterpump vacuum, the residue is stirred with petroleum ether, and the product which is obtained in this process in the form of crystals is isolated by filtering off with suction. 4.9 g (26% of theory) of 7-(2,6-dichloro-4-trifluoromethyl-phenoxy)-2-naphthol of melting point 98 C. are obtained.

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, 3,4,5-Trichlorobenzotrifluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bayer Aktiengesellschaft; US5108489; (1992); 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. 933190-51-3, name is 8-Bromo-6-chloroimidazo[1,2-b]pyridazine, A new synthetic method of this compound is introduced below., HPLC of Formula: C6H3BrClN3

To a stirred solution of phenylmethanol (3.35 g, 31 mmol, 1.2 eq) in THF (80 mL), NaH (60% dispersion in mineral oil, 1.34 g, 33.5 mmol, 1.3 eq) is added in portions. The resulting mixture is stirred at RT for 30 min and then 8-bromo-6-chloroimidazo[1,2-b]pyridazine (D-3) (6 g, 25.8 mmol, 1.0 eq) is added. The resulting mixture is stirred at RT for an additional 2 h and then poured into water (30 mL). The mixture is extracted with ethyl acetate (2*100 mL). The combined organic layers are washed with brine, dried over Na2SO4 and filtered. The filtrate is concentrated in vacuo to afford the product, 8-(benzyloxy)-6-chloroimidazo[1,2-b]pyridazine (D-4).

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; Ren, Pingda; Liu, Yi; Li, Liansheng; Chan, Katrina; Wilson, Troy Edward; Castro, Alfredo C.; Evans, Catherine A.; Snyder, Daniel A.; US2012/122838; (2012); 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. 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C6H3BrClF

1-Bromo-4-chloro-2-fluorobenzene (61g, 291mmol), 2,6-dimethoxyphenylboronic Acid (50.4g, 277mmol), K2CO3 (60.4g, 437mmol) and Pd(PPh3)4 (10.1g, 8.7mmol) were added to a round bottom flask and dissolved in THF (500ml) and distilled water (200ml) and stirred under reflux at 60 C for 12 hours. After completion of the reaction, remove the water layer and perform column chromatography (Hexane: DCM (20%)), by using the intermediate (Int-1) to afford 38g (51%)

The synthetic route of 1996-29-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung SDI Co., Ltd; Samsung Electronics Co., Ltd.; Lee Seung-jae; Kim Chang-u; Kim Byeong-gu; Kim Hyeong-seon; Ryu Dong-wan; Shin Chang-ju; Jang Gi-po; Seo Min-seok; Jeong Seong-hyeon; (39 pag.)KR102044943; (2019); B1;,
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