Month: March 2021

Adding a certain compound to certain chemical reactions, such as: 348-59-4, name is 2,5-Dichlorofluorobenzene, 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 348-59-4, Quality Control of 2,5-Dichlorofluorobenzene

To a solution of 12a (0.200 g; 0.960 mmol) and NMP (4 mL) was added K2CO3 (0.398 g; 2.88 mmol) and 1,4-dichloro-2-fluoro-benzene (0.124 mL; 1.056 mmol). The reaction was heated to 120 C. and monitored by TLC. After 8 h the reaction was cooled to RT and 10% HCl was added. The mixture was extracted with EtOAc and the combined extracts were washed with H2O and brine. The extracts were dried (Na2SO4) filtered and evaporated. The crude product was purified by SiO2 chromatography eluting with a gradient of hexane/EtOAc (100:0 to 60:40) to afford 142.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2,5-Dichlorofluorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Roche Palo Alto LLC; US2005/239881; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 14862-52-3, name is 3,5-Dibromochlorobenzene, 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 14862-52-3, Recommanded Product: 14862-52-3

The following reagents and solvent were charged into a reaction vessel. Tris(dibenzylideneacetone)dipalladium(0): 190 mg (0.21 mmol) Tri(t-butyl)phosphine: 170 mg (0.82 mmol) Toluene: 20 ml. Next, the reaction solution was stirred at room temperature for 15 minutes. After that, the following reagents were charged into the reaction solution. Compound J13: 560 mg (2.1 mmol) Compound J14: 1.0 g (4.6 mmol) t-Butoxysodium: 880 mg (9.1 mmol). Next, the reaction solution was heated to 100 C. and then stirred at the temperature (100 C.) for 3 hours. After the completion of the reaction, the reaction solution was cooled and then an organic layer was extracted with toluene. Next, the extracted organic layer was dried and then the solvent was removed by distillation under reduced pressure to provide a coarse product. Next, the coarse product was purified by silica gel column chromatography (developing solvent; heptane_toluene=3:1) to provide 760 mg (yield: 67%) of Compound J15.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Dibromochlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Canon Kabushiki Kaisha; Nishide, Yosuke; Yamada, Naoki; Kamatani, Jun; Ishii, Ryuji; Kajimoto, Norifumi; Ito, Takayuki; Mizuno, Nobutaka; Ishige, Koichi; Saitoh, Akihito; (71 pag.)US9755165; (2017); B2;,
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. 7464-11-1, name is 5,7-Dichloro-2-methylthiazolo[5,4-d]pyrimidine, A new synthetic method of this compound is introduced below., Computed Properties of C6H3Cl2N3S

To interemdiate 17.6 (123 mg, 0.62 mmol, 1.03 equiv) and compound 23.1 (132 mg, 0.60 mmol, 1.00 equiv) in 2-butanol (5 mL) was added DIEA (155 mg, 1.20 mmol, 2.00 equiv) and the resulting solution was stirred for 4 h at 100 C under nitrogen. The resulting mixture was concentrated under vacuum and crude was purified using flash column chromatography to furnish 160 mg of intermediate 29.1 as a white solid. LCMS (ES, m/z): 382 and 384 [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; NIMBUS IRIS, INC.; ROMERO, Donna L.; MASSE, Craig E.; ROBINSON, Shaughnessy; GREENWOOD, Jeremy Robert; HARRIMAN, Geraldine; WO2015/48281; (2015); 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. 14490-19-8, name is 1,4-Dichloropyrido[3,4-d]pyridazine, A new synthetic method of this compound is introduced below., Application In Synthesis of 1,4-Dichloropyrido[3,4-d]pyridazine

To a 50ml round bottomed flask were added 1 ,4-dichloropyrido[3,4-d]pyridazine (200mg, 1 mmol), potassium carbonate (0.37mL, 2mmol), 2,2,2-trifluoro-N-[[4-fluoro-2-(trifluoromethyl)phenyl]methyl]- N-(4-piperidyl)acetamide (409mg, 1 .1 mmol), NMP (3.OmL) and the reaction was refluxed at 10000overnight. The reaction was cooled and diluted with ethyl acetate. The organic layer was washed with water (5x2OmL). The organic layer was dried (MgSO4) and concentrated in vacuo to afford N- [1 -(1 -chloropyrido[3,4-d]pyridazin-4-yl)-4-piperidyl]-2,2,2-trifluoro-N-[[4-fluoro-2- (trifluoromethyl)phenyl]methyl]acetamide (480mg, 0.9Ommol, 90%) which was used without further purification. MS Method 2: RT: 1 .94mm, m/z 536.2/538.2 [M¡ÂH]

The synthetic route of 14490-19-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; REDX PHARMA LIMITED; ARMER, Richard; BINGHAM, Matilda; BHAMRA, Inder; MCCARROLL, Andrew; WO2014/191737; (2014); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 10061-02-6, name is trans-1,3-Dichloropropene, 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 10061-02-6, Quality Control of trans-1,3-Dichloropropene

To a 3000 mL three-necked flask equipped with a thermometer, a condenser, a constant pressure dropping funnel and a stirrer, 437.2 g (1.0 mol) of fipronil, 60 g (1.5 mol) of NaOH and 1500 mL of ethanol were added, 138.8 g (1.25 mol) of 1,3-trans-dichloropropene was added dropwise at -10 C, and after completion of the dropwise addition, the temperature was controlled at -10 C for 24 hours. The reaction was completed, filtered, the filtrate was adjusted with concentrated hydrochloric acid system pH to neutral, under 40 C vacuum solvent recovery, the residue was slowly added dropwise to ice water, the temperature was controlled at 0 ~ 5 crystallization, filtration, residue by methanol Crystallization, filtration, drying, to give a white crystalline solid 390.0g. Yield 72.8%, liquid chromatography quantitative analysis of content of 95.5%.

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, trans-1,3-Dichloropropene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hunan Chemical Institute Co., Ltd.; Du Shenghua; Lan Shilin; Liu Weidong; Liu Yuan; Huang Chaoqun; Wang Yanli; Luo Liangming; (6 pag.)CN105949126; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 57946-56-2, name is 4-Chloro-2-fluoroaniline, 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. HPLC of Formula: C6H5ClFN

EXAMPLE 35 Preparation of N-(4-Chloro-2-fluorophenyl)-1-cyclohexene-1,2-dicarboximide STR114 A mixture of 4-chloro-2-fluoroaniline (19.0 g, 130.6 mmol), and 3,4,5,6-tetrahydrophthalic anhydride (19.85 g, 130.6 mmol) in acetic acid (150 mL) is refluxed for 2 hours, treated with additional 4-chloro-2-fluoroaniline (3.0 g), refluxed for 90 minutes, stirred at room temperature overnight and poured into a water/ethyl acetate mixture. The organic phase is washed sequentially with water, saturated sodium hydrogen carbonate solution and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a purple oil. Flash column chromatography of the oil using silica gel and 15% to 20% ethyl acetate in hexanes solutions gives the title product as an off-white solid (25.3 g, mp 81-82 C.).

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

Reference:
Patent; American Cyanamid Company; US5679791; (1997); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 6940-78-9, 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. 6940-78-9, name is 1-Bromo-4-chlorobutane belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

1L reaction flask were successively added 7-hydroxy -1H- quinolin-2-one (50g, 0.31mol), ethanol (500 mL) and Sodium hydroxide (20.8g,0.37 mol) was added with stirring 1-bromo-4-chlorobutane (106g, 062 mol). Reaction was heated to reflux and stirred 5h. Down to room temperature and stirred for 30min, and filtered. The filter cake machine water (200 mL) added to the reaction flask and stirred for 30min, and filtered. The filter cake and ethanol (200 mL) added to the reaction flask, was heated to reflux and stirred for LH, cooled to room temperature stirred for 30min, filtered, the filter cake in ethanol (50 mL) washedBrine, and dried in vacuo (50 C) 5h, to obtain 7- (4-chlorobutoxy) -1Eta- quinolin-2-one (6,68.8g, yield 88%)

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, 1-Bromo-4-chlorobutane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shanghai Pharmaceutical Co. Ltd.; Zheng, Yong Yong; Jin, Hua; Zhou, Feng; Huang, Mei Hua; Meng, Xin; (7 pag.)CN105440026; (2016); A;,
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. 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C6H3BrCl2

Compound 6B (42.0 g, 86.60 mmol) and Reagent 4 (19.6 g, 86.60 mmol) were put into 500 ml of tetrahydrofuran under a nitrogen atmosphere, and the resulting mixture was stirred and refluxed. Thereafter, potassium carbonate (35.9 g, 259.79 mmol) was dissolved in 200 ml of water, the resulting solution was introduced into the mixture, the resulting mixture was sufficiently stirred, and then tetrakistriphenyl-phosphinopalladium (3.0 g, 2.6 mmol) was introduced thereinto. After the reaction for 12 hours, the temperature of the product was lowered to normal temperature and a produced solid was filtered. After the filtration, the solid was washed with 200 ml of tetrahydrofuran, 500 ml of ethyl acetate, 500 ml of water, and 300 ml of ethanol. The resulting product was dried to prepare Compound 6C (33.5 g, 77percent). Reagent 4 was purchased from Aldrich.

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:
Patent; LG Chem, Ltd.; Jung, Min Woo; Lee, Dong Hoon; Huh, Jungoh; Jang, Boonjae; Kang, Minyoung; Heo, Dong Uk; Han, Miyeon; (52 pag.)US2018/244630; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

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. Recommanded Product: 4-Bromo-2-chloroaniline

[(1-Ethoxycyclopropyl)oxy](trimethyl)silane (5.6 mL, 27.85 mmol) was added drop wise over 10 minutes to a stirred solution of 4-bromo-2-chloroaniline (5.0 g, 24.22 mmol) in a mixture of methanol (50 mL) and acetic acid (95 mL) and the resulting solution was heated to 70 oC and stirred at this temperature for 4 hours. After this time, the reaction mixture was cooled to room temperature and concentrated. The resulting residue was then dissolved in THF (25 mL) and added drop wise to a cooled (0 oC), stirred solution of sodium borohydride (1.87 g, 49.4 mmol) and (diethyl ether)(trifluoro)boron (6.2 mL, 48.9 mmol) in THF (50 mL). The resulting mixture was then heated to 70 oC and stirred at this temperature for 4 hours before being cooled to room temperature and allowed to stand overnight. The resulting reaction mixture was quenched by the addition of water (100 mL) before being extracted with ethyl acetate (3 x 30 mL). The combined organic extracts were washed sequentially with water (100 mL) and brine (100 mL) before being dried (MgS04), filtered and concentrated. The resulting residue was purified on a Biotage isolera (5% ethyl acetate, 95% heptanes) to give the desired compound (4.8 g, 76% yield) as a colourless oil. Tr = 2.44min m/z (ES+) (M+H+) 246/248.

The synthetic route of 38762-41-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; COURTNEY, Stephen Martin; PRIME, Michael; MITCHELL, William; BROWN, Christopher John; DE AGUIAR PENA, Paula C.; JOHNSON, Peter; DOMINGUEZ, Celia; TOLEDO-SHERMAN, Leticia M.; MUNOZ, Ignacio; WO2013/33085; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 118-69-4,Some common heterocyclic compound, 118-69-4, name is 2,6-Dichlorotoluene, molecular formula is C7H6Cl2, 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.

5 g of the following catalyst particles, as described in examples 3 and 4, were loaded in the reactor along with the diluent corundum particles (1: 1 by weight) and tested the influence of addition of ethyl bromide (2 % VN) in presence and absence of water vapour. The reaction was performed under the following conditions. A reaction temperature of 350 to [400C] was used. The mole ratio 2,6-DCT : H20 : NH3: air: N2 was 1: 15: 3-4: 21: 0-29. Molar concentration of 2,6-DCT is 1.4 to 3.8 %.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,6-Dichlorotoluene, its application will become more common.

Reference:
Patent; TESSENDERLO CHEMIE S.A.; WO2003/101939; (2003); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics