Category: chlorides-buliding-blocks

Reference of 67330-62-5, 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. 67330-62-5, name is 3-Chloro-2,6-diethylaniline, This compound has unique chemical properties. The synthetic route is as follows.

Example 4Synthesis of M-MIPACDEAIn a 5 litre flanged reaction vessel were placed a mixture of 137 ml of sulphuric acid, 580 ml water and 313 ml propan-2-ol. To this were added 250 grams of 3-chloro-2,6-diethylaniline and 203 grams of 2-methyl-6-isopropylaniline. The flask was provided with a stirrer, dropping funnel and condenser and the temperature was raised to 60 C.Formalin solution (35% w/w), 120 ml, was added over a period of 1 hour and heating was subsequently continued for 5 hours. The vessel contents were cooled and neutralised with ammonia solution.The product was extracted into ethyl acetate, washed with water, dried over sodium sulphate, filtered and rotary evaporated to give 467 grams of an amber liquid.Analysis by HPLC showed that the desired hybrid methylene bis-aniline M-MIPACDEA is present at 63% of the total, together with 15% of M-MIPA and 21% of M-CDEA.The liquid showed no sign of crystallisation over 3 months.

The chemical industry reduces the impact on the environment during synthesis 3-Chloro-2,6-diethylaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; HEXCEL COMPOSITES LIMITED; US2012/316262; (2012); A1;,
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. 1303587-99-6, name is 2-Chloro-7,8-dihydro-6H-pyrimido[5,4-b][1,4]oxazine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 2-Chloro-7,8-dihydro-6H-pyrimido[5,4-b][1,4]oxazine

Synthesis of2-chloro-8-(4-(trifluoromethyl) benzyl)-7, 8-dihydro-6H-pyrimido [5, 4-b] [I, 4] [0459] To a stirred solution of 2-chloro-7, 8-dihydro-6H-pyrimido [5, 4-b] [1, 4] oxazine (150 mg, 0.87 mmol) in DMF (3 mL) under argon atmosphere were added sodium hydride (42 mg, 1.75 mmol) and l-(bromomethyl)-4-(trifluoromethyl) benzene (251 mg, 1.05 mmol) at 0 C. The reaction mixture was stirred for 30 min at 0 C. After consumption of the starting materials (monitored by TLC), the reaction was quenched with cold water (20 mL) and extracted with EtOAc (2 x 100 mL). The combined organic extracts were washed with brine (5 mL), dried over sodium sulfate, filtered and concentrated in vacuo. The crude material was washed with n-pentane (2 x 5 mL) to afford 2-chloro-8-(4-(trifluoromethyl) benzyl)-7, 8- dihydro-6H-pyrimido [5, 4-b] [1, 4] oxazine (220 mg, 76%) as an off-white solid. 1H-NMR (OMSO-d6, 500 MHz): delta 7.76 (s, 1H), 7.74 (d, 2H), 7.52 (d, 2H), 4.89 (s, 2H), 4.23-4.20 (m, 2H), 3.57-3.54 (m, 2H); LCMS: 329.8 (M+l); (column; X-Select CSH C-18 (50 3.0 mm, 3.5 mupiiota); RT 3.88 min 0.05% Aq TFA: ACN; 0.80 mL/min); UPLC (purity): 90.0%; (column; Acquity UPLC BEH C-18 2.1 X 50 mm, 1.7 mupiiota); RT 2.58 min. ACN: 0.025% Aq TFA; 0.5 mL/min; TLC: 30% EtOAc/hexane (R 0.4).

According to the analysis of related databases, 1303587-99-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; FORUM PHARMACEUTICALS INC.; BURNETT, Duane, A.; BURSAVICH, Matthew, Gregory; MCRINER, Andrew, J.; WO2015/66697; (2015); 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. 367-22-6, name is 4-Chloro-3-fluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C6H5ClFN

To a solution of 6-acetoxy-7-methoxy-quinazolin4-one (RO0505111-000) (1.0 g, 4.26 mmol) (from Example 15, Step A, supra) in SOCl2 (12.5 mL) (Aldrich) were added a few drops of DMF (0.1 mL). The reaction mixture was then heated with stirring at 100 C. for 3 hours. The solvents were evaporated and the residue was dried in vacuo. The residue was dissolved in 2-propanol (20 mL), followed by addition of 4-chloro-3-fluoroaniline (0.682 g, 4.69 mmol) (Aldrich). The reaction mixture was heated at 110 C. for 3 hours. The reaction mixture was cooled to room temperature and filtered. The precipitate was collected and dried in vacuo to give 6-acetoxy-4-(3-chloro-4-fluoro-phenylamino)-7-methoxy-quinazoline as a gray solid. (Yield 1.54 g, 100%).

The synthetic route of 367-22-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Luk, Kin-Chun; Zhang, Zhuming; US2004/254205; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 1984-58-3,Some common heterocyclic compound, 1984-58-3, name is 1,4-Dichloro-2-methoxybenzene, molecular formula is C7H6Cl2O, 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.

900 mL of ammonia was condensed at -78 C. 1 g of thinly shaven strips of sodium was added followed by 1.0 g of iron (III) nitrate nonahydrate. Upon disappearance of the deep blue color 25 g of thinly shaven strips of sodium was added. After 30 mins of stirring at -78 C., 50 g of 2,5-dichloroanisole was added as a solution in hexane (70 mL) dropwise and the reaction warmed to -45 C. for 2 hrs. Upon completion the ammonia was allowed to evaporate. The crude pot was then diluted in chloroform and 100 g of NH4Cl was added slowly. The combines were taken up in a separatory funnel and washed with water (3*) followed by brine (1*). The organic layer was dried over sodium sulfate and concentrated in vacuo. The resulting solid can be used without further purification. Yield: 99%. 1H NMR (400 MHz, DMSO) delta 6.98 (d, J=8.4, 1H), 6.34 (d, J=1.8, 1H), 6.16 (dd, J=8.4, 1.9, 1H), 5.23 (s, 2H), 3.74 (s, 3H). 13C NMR (101 MHz, DMSO) delta 154.90, 149.16, 129.68, 107.02, 106.74, 98.66, 55.38. HRMS (ESI) calculated for C7H8ClNO [M+H]+: 157.0367. found: 157.0361.

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

Reference:
Patent; Manetsch, Roman; Cross, Richard Matthew; Namelikonda, Niranjan Kumar; Kyle, Dennis Edward; Mutka, Tina Susanna; LaCrue, Alexis Nichole; Maignan, Jordany Richarlson; Saenz, Fabian Ernesto; US2013/123258; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 93-50-5, name is 4-Chloro-2-methoxyaniline, 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 93-50-5, category: chlorides-buliding-blocks

General procedure: Aniline (0.94 g,0.010 mol) was added dropwise, with stirring, to syrupy phosphoricacid (15 mL) at 0C. Finely ground sodiumnitrite (0.83 g,0.012 mol) was added with stirring over 15 min. This solutionwas allowed to stand at 0C for ca. 1 h after which time urea(ca. 100 mg) was added to destroy unreacted nitrite. After a further30min at 0C, a solution of freshly distilledmercaptoaceticacid (0.92 g, 0.010 mol) in water (250 mL) at 0C was addedswiftlywithvigorous stirring,maintainingapHof ca. 4. After ca.1 h of stirring at 0C, a dense pale buff precipitate had formed.The suspension was then filtered, washed with distilled waterand dried in a vacuum desiccator. A second crop of precipitatewas obtainedonkeeping the filtrate for severalhours at 0C. Thecombined dried crops were purified by dissolving in a minimumof dry diethyl ether and adding dry petroleum ether (bp. 40-60C) at 0C. After 1 h at 0C, fine, very pale buff needles wereformed; these were filtered and dried in vacuo to give 1a (1.51 g,77%).

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, 4-Chloro-2-methoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Buglass, Alan J.; Datta, Mrityunjoy; Phosphorus, Sulfur and Silicon and the Related Elements; vol. 193; 4; (2018); p. 218 – 224;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 623-12-1,Some common heterocyclic compound, 623-12-1, name is 1-Chloro-4-methoxybenzene, molecular formula is C7H7ClO, 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 6 The general procedure from Example 1A was followed using 4-chloroanisole (171 mg, 1.2 mmol) and piperidine (100 mul, 1.0 mmol) with Pd2(dba)3 (20 mg, 0.0218 mmol) and (Me3C)2PH(O) (14.5 mg, 0.0878 mmol) and NaOtBu (144 mg, 1.5 mmol) in 4.0 mL of toluene. After 12 h, the reaction mixture was chromatographed with 5% ethyl acetate/hexane to give 128 mg (67% yield) of N-(4-methoxyphenyl)piperidine. It was >95% pure by 1H NMR and GC/MS. 1H NMR (500 MHz, CDCl3): delta 6.81 (d, J=9.11 Hz, 2H), 6.72 (d, J=9.11 Hz, 2H), 3.65 (s, 3H), 2.92 (t, J=5.46 Hz, 4H), 1.60 (m, 4H), 1.46 (m, 2H) ppm. 13C NMR (125 MHz, CDCl3): delta 153.5, 146.8, 118.6, 114.3, 55.4, 52.2, 26.1, 24.1 ppm.

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

Reference:
Patent; Li, George Y.; US2002/137974; (2002); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 1127-85-1, These common heterocyclic compound, 1127-85-1, name is 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline, 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.

The title compound in this step was prepared according to the method described in step 4 of Example 4, ie, 2,4_dichloro_5,6,7,8-tetrahydroquinazoline (3.21 g, 15.8 lmmo 1) and sodium hydroxide solution (100mL, 1mol/L) and tetrahydrofuran (12mL)Reaction at 60C for 12h. The obtained crude product was separated and purified by silica gel column chromatography (petroleum ether/ethyl acetate (nu/nu) = 4/1) to obtain the standardThe title compound (white solid, 2.61g, 91%).

Statistics shows that 2,4-Dichloro-5,6,7,8-tetrahydroquinazoline is playing an increasingly important role. we look forward to future research findings about 1127-85-1.

Reference:
Patent; GUANGDONG HEC PHARMACEUTICAL; Guangdong Dongyangguang Pharmaceutical Co., Ltd.; JIN CHUANFEI; Jin Chuanfei; LAO JINHUA; Lao Jinhua; ZHANG YINGJUN; Zhang Yingjun; (35 pag.)CN108299437; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 445-13-6, 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. 445-13-6, name is 3-Chloro-4-(trifluoromethyl)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of 6 (0.13 mmol, 1 eq) in THF (0.5 mL, 0.26M) in a 1-dram vial at room temperature aniline/heterocyclic amine (0.13 mmol, 1 eq) was added in one portion. The vial was sealed and the mixture heated to reflux for 16 hours to yield crude 7. For compounds 8, after cooling to room temperature, N,N-Diisopropylethylamine (0.143 mmol, 1.1 eq) and isobutyl chloroformate (0.143 mmol, 1.1 eq) were added and the reaction was stirred for 30 minutes at room temperature. For primary carboxamide congeners, ammonium hydroxide (1mL) was added and the reaction was stirred for an additional hour at room temperature. For substituted amide analogs, desired amine (0.26, 2 eq) was added instead of ammonium hydroxide and stirring was continued for an additional 2 hours. The reaction was then diluted with ether (1mL), the layers were separated and the aqueous layer was extracted with ether (3x2mL). The organic layers were passed through a phase separator and concentrated in vacuo, and then crude product was purified using preparative HPLC (30x50mm column, MeCN/0.1% TFA: Water, 4 min gradient) to yield desired compounds 8.

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-Chloro-4-(trifluoromethyl)aniline, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Fulton, Mark Gallant; Loch, Matthew Thomas; Cuoco, Caroline Anne; Rodriguez, Alice Lambert; Days, Emily; Vinson, Paige Newton; Kozek, Krystian Andrezej; Weaver, Charles David; Blobaum, Anna Louise; Conn, Peter Jeffrey; Niswender, Colleen Marie; Lindsley, Craig William; Letters in drug design and discovery; vol. 16; 12; (2019); p. 1387 – 1394;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 7006-52-2, name is N-Methyl-3-chloroaniline, 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. Formula: C7H8ClN

General procedure: To a solution of 13 (500 mg, 1.86 mmol) in DMF (5.0 mL) were added N-methylaniline (241 muL, 2.23 mmol), 1-hydroxybenzotriazole (251 mg, 1.86 mmol) and 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (534 mg, 2.79 mmol) at room temperature. The reaction mixture was stirred at room temperature for 12 h. Water was then added, and the mixture was extracted with a mixture of toluene and EtOAc (1:1). The organic layer was washed with H2O and brine, and dried over anhydrous sodium sulfate. After filtration, the solvent was removed in vacuo, and the residue was purified by silica gel column chromatography using hexane/EtOAc (1:1, v/v) as eluent. The solvent was removed in vacuo, and the resulting solid was recrystallized from iPrOH to give 14 (547 mg, 82percent) as a white solid

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

Reference:
Article; Fukaya, Takayuki; Kodo, Toru; Ishiyama, Takeo; Kakuyama, Hiroyoshi; Nishikawa, Hiroyuki; Baba, Satoko; Masumoto, Shuji; Bioorganic and Medicinal Chemistry; vol. 20; 18; (2012); p. 5568 – 5582;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 104-77-8, 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. 104-77-8, name is 3-Chloro-N,N-diethylpropan-1-amine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 46 3-[1-(3-Diethylaminopropyl)-4-piperidyl]-1,2-benzisoxazole difumarate A suspension of 4.0 g of 3-(4-piperidyl)-1,2-benzisoxazole, 3.2 g of 3-diethylaminopropyl chloride, 3.0 g of potassium iodide and 5.0 g of sodium bicarbonate in 100 ml of butanol was heated under reflux for 2 hrs, cooled to room temperature and filtered. The filitrate was washed with water and extracted with ether (3 times). The ether extracts were dried over anhydrous sodium sulfate, filtered and evaporated to give an oil. The oil was dissolved in 10 ml of acetonitrile and 4.2 g of fumaric acid was added. The mixture was stirred for 2 hrs, filtered and the filter cake was recrystallized three times from ethanol-ether to give 2.8 g (26%) of product, mp 174-176. ANALYSIS: Calculated for C19 H29 N3 O2C4 H4 O4: 59.22%C; 6.81%H; 7.67%N; Found: 59.26%C; 7.01%H; 7.33%N.

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-Chloro-N,N-diethylpropan-1-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Hoechst-Roussel Pharmaceuticals; US4355037; (1982); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics