Category: chlorides-buliding-blocks

Reference of 33050-38-3, These common heterocyclic compound, 33050-38-3, name is 3,6-Dichloro-[1,2,4]triazolo[4,3-b]pyridazine, 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.

b) The 3-chloro[1,2,4]triazolo[4,3-b]pyridazin-6-amine can be prepared in the following way:A mixture of 190 mg of commercial 3,6-dichloro[1,2,4]triazolo[4,3-b]pyridazine and 1 cm3 of aqueous ammonia at 35% in 1 cm3 of dioxane, in a sealed tube, is heated at between 70 C. and 90 C. for 3 1H). The precipitate formed is filtered off, to give 156.4 mg of 3-chloro[1,2,4]triazolo[4,3-b]pyridazin-6-amine in the form of a beige powder, the characteristics of which are as follows:MASS SPECTRUM: UPLC-MS-DAD-ELSD: 168=MH-; 170=MH+.

The synthetic route of 33050-38-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; sanofi-aventis; US2010/298315; (2010); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 51572-93-1, name is O-(2,4-Dichlorobenzyl)hydroxylamine hydrochloride, 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 51572-93-1, Recommanded Product: 51572-93-1

General procedure: A mixture of substituted O-benzylhydroxylamine hydrochloride (1 equiv), TEA (1 equiv) and substituted salicylaldehyde (1 equiv) was dissolved in absolute ethanol and stirred for 0.5 h. The reaction was monitored by TLC. The precipitate was filtered and recrystallized from ethanol to gain salicylaldoxime (compounds 1g-20g).

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, O-(2,4-Dichlorobenzyl)hydroxylamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Zhao, Ting-Ting; Lu, Xiang; Yang, Xian-Hui; Wang, Li-Ming; Li, Xi; Wang, Zhong-Chang; Gong, Hai-Bin; Zhu, Hai-Liang; Bioorganic and Medicinal Chemistry; vol. 20; 10; (2012); p. 3233 – 3241;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 139512-70-2, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 139512-70-2 name is 4-Chloro-5-fluorobenzene-1,2-diamine, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

4-Chloro-5-fluoro-benzene-1,2-diamine (5.20 g; 32.4 mmoles) and 3,3,3-trifluoro-2-hydroxy-propionic acid (7.00 g; 48.6 mmoles) were suspended in 6N HCl (9 mL; 54 mmoles) under a nitrogen atmosphere. The reaction was stirred vigorously and heated to 108C for 18 hrs, then cooled to room temperature. The reaction was diluted with water (100 mL) and with ethyl acetate (100 mL), then sodium bicarbonate (6.90 g; 81.00 mmoles) was added slowly and in portions to quench the reaction. The aqueous layer was separated and extracted with ethyl acetate (3×40 mL). The extracts were combined, washed with water (30 mL) and brine (30 mL), then dried over Na2SO4. The filtrate was concentrated in vacuo to yield a crude brown solid which was then purified by column chromatography (SiO2; 30% ethyl acetate/CH2Cl2) to yield the title compound as an off-white solid. 1H NMR (400 MHz, CD3CN) delta 7.74 (d, J = 6.7 Hz, 1 H), delta 7.49 (d, J =9.5,1 H), delta 5.41 (q, J = 6.8 Hz, 1 H), delta 5.16 (br s, 1 H), delta 2.35 (s, 6H) MS calculated for C9H5ClF4N2O: 268.00 MS measured: 269 (M+H); 267 (M-H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-5-fluorobenzene-1,2-diamine, and friends who are interested can also refer to it.

Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2006/39243; (2006); 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. 627-42-9, name is 2-Methoxyethyl chloride, A new synthetic method of this compound is introduced below., name: 2-Methoxyethyl chloride

2,5-Di-tert-butylhydroquinone (0.2 mmol) was dissolved in anhydrous THF (20 ml). Sodium hydride (0.6 mmol) and 2-chloroethylethylether (0.4 mmol) was then added to the solution. The reaction mixture was then stirred at room temperature overnight. After removal of the solvent, the residue was partitioned between dichloromethane and aqueous NaHCO3 (0.1M). The organic portion was separated and dried over Na2SO4. After solvent removal in vacuo, the crude product was chromatographed (silica, hexanes/DCM from 5:1 to 1:1) to afford 1,4-bis(2-methoxyethoxy)-2,5-di-tert-butyl-benzene in an 81% yield. The product was characterized by 1H NMR (300 MHz, CDCl3, delta/ppm): 7.14 (s, 2H), 4.11 (t, J=4.5 Hz, 4H), 3.80 (t, J=4.5 Hz, 4H), 3.45 (s, 6H), 1.37 (s, 18H).

The synthetic route of 627-42-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhang, Zhengcheng; Zhang, Lu; Amine, Khalil; US2011/294003; (2011); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 626-43-7, A common heterocyclic compound, 626-43-7, name is 3,5-Dichloroaniline, molecular formula is C6H5Cl2N, 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.

In a reaction flask, 48 g (0.3 mol) of 3,5-dichloroaniline was added to a mixed solution of 500 mL of water and 500 mL of hydrochloric acid.Medium, after stirring evenly, cool down to 0 C,Under stirring, 400 mL of an aqueous solution containing 23 g (0.34 mol) of sodium nitrite was added dropwise, and after mixing, the mixture was uniformly mixed to obtain a solution A;1000 mL of an aqueous solution containing 67 g (1.2 mol) of potassium hydroxide was placed in another reaction flask.Under the condition of 0 C, slowly add 250 mL of ethanol (35 mol) dissolved in ethyl pyruvate, and then add to the solution B after stirring.After the solution A was brought to a temperature of 0 C, the solution B was slowly added dropwise to the solution A, and after the completion of the dropwise addition, the temperature was raised to 40 C for 10 minutes, and then the reaction solution was extracted three times with 1000 mL of diethyl ether.The organic phases were combined, dried over anhydrous magnesium sulfate (100 g), concentrated, and then recrystallized from a mixture of n-hexane and acetone (V-hexane: Vacetone = 2:1) to give ethyl-2-(2-(3,5-) Chlorophenyl)indenyl)propionic acid 78g,Yield is 95%

The synthetic route of 626-43-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Henan Wanliu Biological Technology Co., Ltd.; Yang Weixiao; Ren Baoqi; Wang Jiahao; (13 pag.)CN108864089; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 367-22-6, name is 4-Chloro-3-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. COA of Formula: C6H5ClFN

Description 45 (78 mg, 0.37 mmol) and 3-fluoro-4-chloroaniline (54 mg, 0.37 mmol) inMeCN (2 ml) in the presence of a catalytic quantityof DMAP were stirred at 45 C for 16 h. The reaction was cooled and the resultant solid collected by filtration and rinsed with ether. Without further purification this solid was added to sodium hydroxide solution(1 % aqueous w/w, 2 ml) and heated at 80 OC for 30 min. The reaction was cooled, filtered throughCeliteX to remove insoluble impurities and the filtrate was acidified to pH-6 by the dropwise addition of hydrochloric acid (5N) to precipitate the product. The solid was collected by filtration, rinsed with water then ether and dried to give the title compound (70 mg). 1H NMR (400 MHz, DMSO)8 7.86(1H, s), 7.70(1H, t, J8.4), 7.43(1H, dd,J2. 2,10. 0), 7.14-7. 12(1H, m),3. 77 (3H, s) ;Mlz (ES+) 313,311 (M+H+).

The synthetic route of 4-Chloro-3-fluoroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MERCK SHARP & DOHME LIMITED; HOLLINGWORTH, Gregory, John; JONES, A., Brian; SPAREY, Timothy, Jason; WO2005/49613; (2005); 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. 13918-92-8, name is 2,4-Difluorobenzene-1-sulfonyl chloride, A new synthetic method of this compound is introduced below., Product Details of 13918-92-8

2,4-Difluorobenzenesulfonyl chloride (4 g, 18.81 mmol) in DCM (10 mL) was added slowly to a solution of 2-(methylamino)ethanol (1.66 mL, 20.70 mmol) in DCM (200 mL) and 10% sodium hydroxide solution (200 mL) at O0C. The reaction was allowed to warm to RT and stirred for 20 hours. The DCM layer was separated and the aqueous re-extracted into DCM (2 x 50 mL). The combined organics were washed with brine, dried (MgSO4), filtered and reduced in vacuo to give the desired compound as a colourless oil (4.7 g). 1H NuMR delta (CDCl3): 1.98 (t, IH), 2.94 (s, 3H), 3.32 (t, 2H), 3.79 (q, 2H), 6.94 – 7.03 (m, 2H), 7.89 – 7.95 (m, IH)

The synthetic route of 13918-92-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/125972; (2006); 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. 7149-75-9, name is 4-Chloro-3-methylaniline, A new synthetic method of this compound is introduced below., Computed Properties of C7H8ClN

Step 1 (0407) To a mixture of 3-formylbenzoic acid methyl ester (1.25 g), 4-chloro-3-methylphenylamine (1.29 g), tetrahydrofuran (15 mL) and methanol (15 mL) was added decaborane (232 mg), and the mixture was stirred at room temperature for 2 hours. After the mixture was diluted with ethyl acetate, to the resulting mixture was added aminopropyl silica gel powder (5 g). The resulting mixture was filtered and the filtrate was concentrated under reduced pressure to give 3-[(4-chloro-3-methylphenylamino)methyl]benzoic acid methyl ester (2.13 g).

The synthetic route of 7149-75-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kissei Pharmaceutical Co., Ltd.; Inoue, Hitoshi; Ohno, Kohsuke; Nakamura, Tetsuya; Ohsawa, Yusuke; (58 pag.)US2016/362368; (2016); 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. 622-86-6, name is (2-Chloroethoxy)benzene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of (2-Chloroethoxy)benzene

2-(4-Aminophenyl) butanoic acid (Compound 10, step 1) (397.3 mg, 2.0 mmol) was suspended with stirring intrifluoroacetic anhydride (277.4 uL, 2.0 mmol). Then (2-chloroethoxy)benzene(252.4 uL, 1.8 mmol) was added dropwise and the resulting mixture was stirredat room temperature overnight. The reaction was quenched with saturated sodiumbicarbonate solution (5 mL) and extracted with ethyl acetate (2 x 15 mL). The combined organic layers were dried overanhydrous magnesium sulfate and concentrated on a rotary evaporator. The resulting residue was purified byreverse-phased chromatography (C-10 column, gradient of acetonitrile in waterwith 0.1% formic acid) to afford 297.1 mg (49%) of the desired product as ayellow solid. 1H NMR (400MHz, MeOD) delta 7.99 (d, J = 8.9 Hz, 2H), 7.28 (m, 4H), 6.96 (d, J = 8.9 Hz, 2H),4.58 (t, J = 7.2 Hz,1H), 4.27 (t, J = 5.5 Hz, 2H), 3.84 (t, J = 5.5 Hz, 2H),2.11 (m, 1H), 1.78 (m, 1H), 0.88 (t, J = 7.3 Hz 3H); MS (ESI) (m/z) 318.1/320.1(M+H)+.

The synthetic route of 622-86-6 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Childers, Wayne; Fan, Rong; Martinez, Rogelio; Colussi, Dennis J.; Melenski, Edward; Liu, Yuxiao; Gordon, John; Abou-Gharbia, Magid; Jacobson, Marlene A.; Bioorganic and Medicinal Chemistry Letters; vol. 30; 2; (2020);,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

849367-49-3, name is 3-Bromo-4-chlorobenzylamine, 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. Recommanded Product: 849367-49-3

Example 120 N1-[(3-Bromo-4-chlorophenyl)methyl]-N1-{[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-1,1-cyclopropanedicarboxamide A mixture of 1-[({[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)carbonyl]cyclopropanecarboxylic acid (600 mg, 1.444 mmol), HBTU (657 mg, 1.733 mmol), Et3N (1006 muL, 7.22 mmol) and 1-(3-bromo-4-chlorophenyl)methanamine (350 mg, 1.589 mmol) in DCM was stirred at room temperature overnight. The reaction mixture was quenched with saturated NaHCO3 and extracted with DCM twice. The combined organic layers were washed with brine and then concentrated under vacuum to give the crude residue. It was then purified with a Gilson HPLC (acidic conditions: 0.1% TFA in the solvents), eluding with 10 to 70% CH3CN in water at a flow rate of 20 mL/min. The product fractions were combined and washed with saturated NaHCO3 and extracted with ethyl acetate twice. The combined organic layers were dried over sodium sulfate, filtered and then concentrated under vacuum to give N1-[(3-bromo-4-chlorophenyl)methyl]-N1-{[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-1,1-cyclopropanedicarboxamide (20 mg, 2.24%). LC-MS m/z 617 M+, 0.92 min (ret time).

The synthetic route of 849367-49-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Glaxo Group Limited; US2009/203677; (2009); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics