Tag: M.W=200-300

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. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, A new synthetic method of this compound is introduced below., Computed Properties of C6H3BrClF

4-Bromo-2-chloro-l-(2-cyano-2-methyl)ethylbenzeneTo a solution of the 4-bromo-2-chloro-l-fluorobenzene (2.1Og, 10.0 mmol) in toluene (15 mL) was added the isobutyronitrile (3.64 mL) followed by KHMDS (0.5 M solution in toluene, 15 mL, 7.50 mmol). Reaction heated at 60 0C for 10 mins and then cooled to 0 0C, poured into IM HCl (5 mL) and extracted with ethyl acetate (2 x 30 mL), orgs washed with brine (10 mL), dried over magnesium sulphate, filtered and concentrated in vacuo. Residue was purified by flash column chromatography (silica, 0 to 50 % EtOAc / hexanes) to yield a brown solid (970 mg, 38%). MS (+ve ESI) : Rt = 2.46 min, no mass ion (M+H)+ 1H NMR (400.132 MHz, CDC13) delta 1.85 (6H, s),7.35 (IH, d),7.43 (IH, m),7.61 (IH, d)

The synthetic route of 60811-21-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2009/1127; (2008); 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. 1996-30-1, name is 3-Bromo-4-fluorochlorobenzene, A new synthetic method of this compound is introduced below., SDS of cas: 1996-30-1

1 -(4-Chloro-2-(trimethylstannyl)phenyl)- 1 H- 1 ,2,4-triazole Step 1. 1 -(2-Bromo-4-chlorophenvD- 1 H- 1 ,2,4-triazole. To a mixture of 2-bromo-4-chloro-l- fluorobenzene (2 g, 9.6 mmol) and 4H-l ,2,4-triazole (0.79 g, 1 1.5 mmol) in DMF (20 mL) was added K2C03 (5.28 g, 38.2 mmol), and the mixture was stirred at 100C for 16 h. The mixture was diluted with water (50 mL) and extracted with EtOAc (50 mL x 3). The combined organic layers were dried over magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel gradient chromatography (Si02, petroleum ether: EtOAc = 10: 1-1 : 1) to give the title compound. 1H NMR (CDC13, 400MHz): delta 8.48 (s, 1H), 8.14 (s, 1H), 7.77 (s, 1H), 7.46 (d, J=l . l Hz, 2H).

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; MERCK SHARP & DOHME CORP.; LIU, Weiguo; EDMONDSON, Scott, D.; GUO, Zhuyan; MERTZ, Eric; OGAWA, Anthony, K.; SO, Sung-Sau; SUN, Wanying; BROCKUNIER, Linda, L.; ALI, Amjad; KUANG, Rongze; WU, Heping; WO2015/183709; (2015); A1;,
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Related Products of 1435-50-3, 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. 1435-50-3, name is 2-Bromo-1,4-dichlorobenzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

25.4 g of 2-bromo-1,4-dichlorobenzene, 8.9 ml of iodoethane and 13.3 ml of DMPU are dissolved in 230 ml of THF, and a solution of 16.2 g of lithium tetramethylpiperidide in THF is added dropwise at -70 C. After a further 2 h at -70 C., the reaction mixture is allowed to warm to ambient temperature, and the batch is hydrolysed using water and worked up by extraction. The crude product is purified by fractional distillation. [0126] b.p.: 73 C./0.1 bar. Colourless liquid.

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

Reference:
Patent; MERCK PATENT GMBH; Reiffenrath, Volker; Jasper, Christian; Manabe, Atsutaka; Montenegro, Elvira; Pauluth, Detlef; US2013/221274; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 1996-29-8,Some common heterocyclic compound, 1996-29-8, name is 1-Bromo-4-chloro-2-fluorobenzene, molecular formula is C6H3BrClF, 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.

Add Intermediate 18 (Int-18) (39.6 g, 134 mmol),1-bromo-4-chloro-2-fluorobenzene (28 g, 134 mmol), K2 CO3 (37 g, 267 mmol) and Pd (PPh3) 4 (4.6 g, 4 mmol) were dissolved in 180 ml of distilled water and 650 ml of THF in a round bottom flask, and then refluxed and stirred at 60 C for 12 hours.When the reaction is complete, the resultant is poured into an excess of methanol,And the obtained mixture was stirred at room temperature for 30 minutes.The solids were filtered, dried and processed by column chromatography (hexane: DCM (30%)).To obtain 26 g (65%) of Intermediate 19 (Int-19).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-4-chloro-2-fluorobenzene, its application will become more common.

Reference:
Patent; Samsung Sdi Co Ltd; Kim, Changwoo; Lee, Seungjae; Kim, Hyung Sun; Ryu, Dong Wan; Shin, Chang Ju; Jang, Kipo; Jung, Sung Hyun; Jung, Juyeon; Chu, Handong; (79 pag.)TW2019/30299; (2019); 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. 13745-86-3, name is 11-Chlorodibenzo[b,f][1,4]thiazepine, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

EXAMPLE 2:PREPARATION OF 11 -PIPERAZINYL DIBENZO[b, f] [1,4] THIAZEPINE A mixture of 1000 ml of organic layer containing product (obtained from example 1) and 1 13.84 grams of Piperazine (1.32 mol) is stirred at 110-120 degree C for about 8 hours. The reaction mass is cooled to 30-35 degree C and washed with water (1×1000 ml and 2×500 ml) Organic layer is dried using Dean stark by azeotropic distillation and taken for next step. Volume of Organic layer is about 1000 ml; Purity (HPLC) : 99.0 %

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; SANDOZ AG; WO2007/20011; (2007); 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. 32943-25-2, name is 3-Chloro-10,11-dihydro-5H-dibenzo[b,f]azepine, A new synthetic method of this compound is introduced below., Safety of 3-Chloro-10,11-dihydro-5H-dibenzo[b,f]azepine

Example 11 2-(4-(3-(3-Chloro-10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)-1-propyl)-1-piperazinyl)-3-pyridinecarboxylic acid dihydrochloride STR17 To a solution of 3-chloro-10,11-dihydro-5H-dibenzo[b,f]azepine (5.0 g, 22 mmol) in toluene (20 ml), 3-chloropropionyl chloride (3.32 g, 26 mmol) in toluene (8 ml) was added dropwise. The reaction mixture was stirred at 95 C. for 2 h and left stirring at room temperature overnight. 2 N Sodium hydroxide (25 ml) followed by toluene (50 ml) were added, and the phases were separated. The toluene phase was washed with 2 N sodium hydroxide (2*25 ml), water (3*30 ml) and brine (30 ml). The organic phase was dried (MgSO4) and evaporated in vacuo. The residue was stripped with methanol (30 ml) and the residue was suspended in ethyl acetate (8 ml), stirred and filtered off. The solid was washed with ethyl acetate (10 ml) and dried. This afforded 4.0 g (57%) of 3-chloro-1-(3-chloro-10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)propan-1-one

The synthetic route of 32943-25-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Novo Nordisk A/S; US5916889; (1999); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 13745-86-3, name is 11-Chlorodibenzo[b,f][1,4]thiazepine, 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 13745-86-3, Quality Control of 11-Chlorodibenzo[b,f][1,4]thiazepine

Example 8 1-piperazinyldibenzo[b,f][1,4]thiazepine A 1 liter round bottom flask equipped with stirring rod, thermo pocket, water condenser was charged with solution of 11-chlorodibenzo[b,f][1,4]thiazepine in toluene [52 gm (0.22 moles)], and the mixture was stirred for 15 min 45-50 C. To the resulting solution was added piperazine 73.0 (0.84 moles) at 45-50 C. The reaction mixture was heated to 70-80 C. The reaction mixture was maintained at 70 C. to 80 C. for 120-180 min. The reaction mixture was analyzed by HPLC (to check for absence of compound of formula III) and was cooled to 20 C. to 25 C. The reaction mixture was added 250 cc DM water and was stirred for 30 min. at 25-30 C. The layers were separated and the organic layer washed with 250 cc DM water. The organic phase was distilled off under vacuum below 70 C. Traces of toluene were removed by adding n-butanol. To the resultant oily mass was added 150 cc n-butanol. The mixture was stirred for 24 hrs and chilled to 0-5 C. The reaction mass was filtered with the filtrate (mother liquor) containing 11-piperazinyldibenzo[b,f][1,4]thiazepine. Purity of 11-piperazinyldibenzo[b,f][1,4]thiazepine in toluene was more than 98.0% (area % by HPLC).

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; Kansal, Vinod Kumar; Ahmad, Suhail; Lal, Kanhaiya; Patil, Bhatu Tumba; US2008/241949; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 33863-76-2, The chemical industry reduces the impact on the environment during synthesis 33863-76-2, name is 1-Bromo-3-chloro-5-fluorobenzene, I believe this compound will play a more active role in future production and life.

To a solution of ethyl 4-ethyl-3-hydroxyphenylacetate (12a, 0.700 g; 3.36 mmol) and NMP (8 mL) was added K2CO3 (1.393 g; 10.08 mmol) and 1-bromo-3-chloro-5-fluorobenzene (59b, 0.774 g; 3.7 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 chromatographed with silica gel and eluted with a gradient of hexane/EtOAc (100 to 60% hexane) to afford 124a.

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-3-chloro-5-fluorobenzene, other downstream synthetic routes, hurry up and to see.

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

Electric Literature of 344-65-0, 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. 344-65-0, name is 1-Bromo-4-chloro-2-(trifluoromethyl)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A 1,4-Dioxane solution (8 mL) of 10 (1.0 mmol), arylboronic acid 2 (1.0 equiv.), K3PO4, and Pd(PPh3)4 (5 molpercent) was heated at 75 C for 4 h. After cooling to room temperature, H2O was added and the reaction mixture was extracted with CH2Cl2. The organic layer was dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified by column chromatography (pure n-heptane).#10;#10;#10;#10;#10;#10;#10;

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

Reference:
Article; Ali, Iftikhar; Siyo, Baraa; Hassan, Zahid; Malik, Imran; Ullah, Ihsan; Ali, Asad; Nawaz, Muhammad; Iqbal, Jamshed; Patonay, Tama?s; Villinger, Alexander; Langer, Peter; Journal of Fluorine Chemistry; vol. 145; (2013); p. 18 – 34;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 50594-82-6,Some common heterocyclic compound, 50594-82-6, name is 3,4,5-Trichlorobenzotrifluoride, molecular formula is C7H2Cl3F3, 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.

(d) 1,3-Bis(2,6-dichloro-alpha,alpha,alpha-trifluoro-p-tolyloxy)benzene A mixture of 3,4,5-trichloro-alpha,alpha,alpha-trifluoro-toluene (10 g. 0.04 mol), and the dipotassium salt of 1,3-dihydroxybenzene (4 g. 0.021 mol) in 150 ml. sulfolane is stirred and heated 70 minutes at ~120 C. The cooled reaction mixture is diluted with benzene (350 ml.) and washed once with water (1 1). Hexane (200 ml.) is added, and the solution washed with water (3*500 ml.) dried, filtered through activated silica gel (~25 g.), and the solvents removed. The residual oil is crystallized from a mixture of pentane and benzene to give 1,3-bis(2,6-dichloro-alpha,alpha,alpha-trifluoro-p-tolyloxy)benzene (5.3 g. 49%) m.p. 121-122 C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,4,5-Trichlorobenzotrifluoride, its application will become more common.

Reference:
Patent; Rohm and Haas Company; US4419122; (1983); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics