Tag: M.W=100-200

Reference of 626-43-7, These common heterocyclic compound, 626-43-7, name is 3,5-Dichloroaniline, 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 5; Preparation of 1,3,5-triaminobenzene from 3,5-dichloroaniline, hydrolysis with hydrochloric acid of the 1,3,5-triaminobenzene to phloroglucinol; A pressurized vessel is charged with 30 g (18.6 mmol) of 3.5-dichloroaniline and 1.8 g of copper iodide in 160 ml of 28% aqueous ammonia. The mixture is heated at 190 C. and under a pressure of 40 bars for 24 h. The contents of the vessel are poured into 200 ml of water and then the excess ammonia is removed. Then 56 g of 10 N hydrochloric acid are added and the mixture is heated at 110 C. for 20 h. Following filtration, the solution is cooled in an ice bath until the phloroglucinol precipitates. The precipitate obtained is subsequently recrystallized from 400 ml of a water-methanol (95 V-5 V) mixture.

Statistics shows that 3,5-Dichloroaniline is playing an increasingly important role. we look forward to future research findings about 626-43-7.

Reference:
Patent; PHV ANALYITIC; US2005/165256; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 4584-46-7, The chemical industry reduces the impact on the environment during synthesis 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, I believe this compound will play a more active role in future production and life.

A solution of 5-nitroindoline (6) (0.5 g, 3.05 mmol) in DMF (10 mL) was treated with NaH (0.39 g, 9.75 mmol, 60% wt in mineral oil) at 0 C resulting in an orange mixture. ;The reaction mixture was then treated with 2-chloro-N,N-dimethylethanamine hydrochloride (0.87 g, 6.09 mmol) resulting in a dark red mixture. ;The reaction was heated to 90 C and stirred for 1.5 h. ;After allowing the reaction to cool to room temperature, water was added and the product was extracted into EtOAc. ;The combined ethyl acetate layer was washed with water, brine and dried (Na2SO4). ;Solvent was evaporated and the crude was purified by flash column chromatography (2 M NH3 in MeOH:CH2Cl2, 2.5:97.5) to obtain the title compound (0.4 g, 56%) as a solid. 1H NMR (DMSO-d6) delta 7.96 (dd, 1H, J = 2.1, 8.7 Hz), 7.79 (d, 1H, J = 2.1 Hz), 6.49 (d, 1H, J = 9.0 Hz), 3.72 (t, 2H, J = 8.7 Hz), 3.39 (t, 2H, J = 6.6 Hz), 3.04 (t, 2H, J = 8.7 Hz), 2.44 (t, 2H, J = 6.3 Hz), 2.18 (s, 6H).

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

Reference:
Article; Annedi, Subhash C.; Maddaford, Shawn P.; Ramnauth, Jailall; Renton, Paul; Rybak, Taras; Silverman, Sarah; Rakhit, Suman; Mladenova, Gabriela; Dove, Peter; Andrews, John S.; Zhang, Dongqin; Porreca, Frank; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 94 – 107,14;; ; Article; Annedi, Subhash C.; Maddaford, Shawn P.; Ramnauth, Jailall; Renton, Paul; Rybak, Taras; Silverman, Sarah; Rakhit, Suman; Mladenova, Gabriela; Dove, Peter; Andrews, John S.; Zhang, Dongqin; Porreca, Frank; European Journal of Medicinal Chemistry; vol. 55; (2012); p. 94 – 107;,
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. 2106-04-9, name is 3-Chloro-2-fluoroaniline, A new synthetic method of this compound is introduced below., Quality Control of 3-Chloro-2-fluoroaniline

3.25 ml phosphorus oxychloride are added dropwise to 6.50 g 6-(1,4-dioxa-spiro[4.5]dec-8-yloxy)-7-methoxy-3H-quinazolin-4-one in 65 ml acetonitrile under an argon atmosphere. Then the reaction mixture is heated to 40 C., combined dropwise with 5.00 ml triethylamine and refluxed for 2 h. After cooling to ambient temperature 1.40 ml triethylamine and 2.60 ml 3-chloro-2-fluoro-aniline, dissolved in 5 ml acetonitrile, are added and the reaction mixture is stirred overnight at 40 C. Then a further 0.70 ml of 3-chloro-2-fluoro-aniline dissolved in 2 ml acetonitrile are added dropwise and the reaction mixture is stirred for a further 10 h. After cooling to ambient temperature the precipitate formed is suction filtered, taken up in 1 N hydrochloric acid, combined with 6 N isopropanolic hydrochloric acid and stirred at ambient temperature until the ketal cleaving is complete. The precipitate formed is suction filtered and combined with methylene chloride and 1 N sodium hydroxide solution. The aqueous phase is separated off and extracted with methylene chloride, the combined extracts are evaporated down and the flask residue is brought to crystallisation with diisopropylether.Yield: 5.90 g (73% of theory)Mass spectrum (ESI+): m/z=416, 418 [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; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2011/46148; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 59681-66-2, These common heterocyclic compound, 59681-66-2, name is 4-Chloro-N1-methylbenzene-1,2-diamine, 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 35 Preparation of 7-Chloro-4,9-dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one A 532 mg. portion of 7-chloro-1,3,4,9-tetrahydro-4-methyl-10H-thieno[3,4-b] [1,5]benzodiazepin-10-one (prepared by the reaction of 4-chloro-2-amino-N-methylaniline and 3-keto-4 -carbomethoxy tetrahydro thiophene at relfux temperature in tolune) is suspended in 4 ml. of pyridine. A 276 mg. portion of N-chlorosuccinimide is added in portions while rinsing with 1 ml. of pyridine. The mixture is heated on a steam bath for 15-20 minutes, cooled and diluted with water yielding a brown solid which is recrystallized twice from methanol yielding 0.25 g., m.p. 244-246C.

The synthetic route of 59681-66-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; American Cyanamid Company; US3953430; (1976); A;,
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

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

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

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

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

108-70-3, name is 1,3,5-Trichlorobenzene, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Application In Synthesis of 1,3,5-Trichlorobenzene

Synthesis Example 5 Synthesis of 1,3,5-Trichloro-2,4,6-tris(phenylethynyl)benzene (corresponding to Scheme 3-(8)) [Show Image] Under a nitrogen atmosphere, in a 100 mL three-neck flask, 1,3,5-trichloro-2,4,6-triiodobenzene (5.0 g, 8.94 mmol) obtained in Synthesis Example 1, diisopropylamine (4.5 mL) and THF (40 mL) were placed and degassed by Ar bubbling for 30 minutes. Pd(PPh3)4 (200 mg, 0.17 mmol), CuI (310 mg, 1.6 mmol) and ethynyl benzene (3.92 mL, 35.8 mmol) were added and refluxed for 20 hours. After the reaction was terminated with a 1N hydrochloric acid solution (20 mL), the reaction mixture was extracted with methylene chloride (50 mL x 3), washed with an aqueous sodium hydrogen carbonate solution (150 mL x 1) and saturated saline solution (150 mL x 2) and dried over anhydrous magnesium sulfate. After the solvent was distilled away under reduced pressure, a by-product(s) was removed by column chromatography (silica gel, hexane, butch) and purification was performed by column chromatography (silica gel, hexane: methylene chloride = 10:1, Rf = 0.38). The resultant solid substance was dissolved in hot benzene and reprecipitated from hexane to obtain a white solid substance (3.3 g, 77%). 1H-NMR(400MHz,CDCl3)delta7.64-7.60(m,6H), 7.42-7.35(m,9H); 13C-NMR(99.5MHz,CDCl3)delta138.1,132.1, 129.5, 128.6, 123.1., 122.4, 101.1, 83.3; M.S.(70eV,EI)m/z=482(M+); mp186.8-187.3C

The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hiroshima University; Nippon Kayaku Kabushiki Kaisha; EP2361915; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics