Tag: M.W=100-200

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;,
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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,
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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;,
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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;,
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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,
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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. 367-22-6, name is 4-Chloro-3-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., Formula: C6H5ClFN

Compound 102[00318] 4-Chloro-3-fluoroaniline; (250.3g, 1.719mol) was added to a 5L four-neck round bottom flask equipped with overhead stirrer, reflux condenser, heating mantle, temperature controller, an internal temperature probe and an argon inlet. r°-Heptane (2000ml) and di-t- butyl-dicarbonate (450.3g, 2.064mol) were charged to the flask. The mixture was stirred under argon at room temperature for 15min allowing dissolution of the majority of the solids. The mixture was heated to reflux for 4h under argon (care: generation of CO2 g). Analysis of the reaction mixture by HPLC method Test 20 (THFrMeCN 1 :1) indicated complete conversion of starting material (Rt 4.57min) to one product (Rt 6.17min). [00319] The reaction was allowed to cool to 50-550C and transferred in two portions to a 3 L one-neck RBF. A total of 1500ml of distillate was removed by concentration in vacuo at 450C to give a peach colored solution with white crystals. The slurry was allowed to cool to room temperature, whilst stirring, for 1.5h. The flask was stored at 40C for 15h after which time the crystals were filtered under vacuum and washed with cold «-heptane (400ml). [00320] After drying at 350C under vacuum for 7h, very fine, white crystals of Compound 102 (393.1g, 93% yield) were obtained. Compound 102: C?Hi3ClFNO2 245.68gmol”. HPLC analysis (Test 20, MeCN): R1 6.16min; 99% purity (at) 254nm. m.p.: 103-1040C. 1H NMR OH (400 MHz, CDCl3): 1.51 (9H, s, 3 x CH3), 6.56 (IH, br-s, N-H), 6.94, 7.25, 7.35 (3 x 1Eta, 3 x m, 3 x Ar-H).

According to the analysis of related databases, 367-22-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; IDENIX PHARMACEUTICALS, INC.; WO2008/42240; (2008); A2;,
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. 94-97-3, name is 5-Chloro-1H-benzo[d][1,2,3]triazole, A new synthetic method of this compound is introduced below., COA of Formula: C6H4ClN3

4-Nitro-5-chloro-1H-benzotriazole [22] 5-Chloro-1H-benzotriazole (3.08g, 20mmol) was dissolved in conc. sulphuric acid (40ml) and cooled to 0C on an ice bath. Nitric acid (40ml, excess) was added drop wise to the cooled solution over a period of 20 minutes. Stirring was continued for 1 hour at 0C and then at 60C for an additional 1 hour, by which time TLC (A) indicated the conversion of starting material. The solution was cooled to room temperature and poured over ice to precipitate a white solid. The solid was collected by filtration and washed with copious amounts of water until neutral to afford [22] in 83% yield. Rf(A) 0.49 deltaH(400MHz; DMSO-d6) 7.75 (1H, d, J8.8, BT) 8.38 (1H, br s, BT); m/z (EI-HR) 197.99383 [(M) calc. for C6H3N4O235Cl 197.99445] and 199.99345 [(M) calc. for C6H3N4O2 37Cl 199.99150].

The synthetic route of 94-97-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; University of Strathclyde; EP1272827; (2008); B1;,
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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. Product Details of 367-22-6

To 4-chloro-3-fluoroaniline (25g, 0.17 mmol) in 250 mL of H20 was added NaHC03 (21.6g, 0.25 mmol). After cooling to 0 C, iodine (43.5 g, 0.17 mmol) was added. After 18 h at rt, an additional 10.8 g of iodine was added and the reaction was stirred overnight. The reaction was extracted with DCM (4×250 mL), the combined organics were washed with sodium thiosulfate solution (2×250 mL) and brine (2×250 mL) and dried ( a2S04). Purification by silica gel chromatography gave 47 g of Intermediate 5A.MS (ESI) m/z: 145.2 (M+H)+.

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

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ORWAT, Michael J.; PINTO, Donald J.P.; SMITH II, Leon M.; SRIVASTAVA, Shefali; CORTE, James R.; WO2013/55984; (2013); A1;,
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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. 2106-02-7, name is 2-Chloro-4-fluoroaniline, This compound has unique chemical properties. The synthetic route is as follows., name: 2-Chloro-4-fluoroaniline

General procedure: To a well stirred solution of compound 6a or 6b (0.2 g, 1 Eq.) in absolute ethanol (10 mL), the appropriately substituted anilines(1.1 Eq) was added and the reaction mixture was refluxed for 2-3 h until TLC showed full consumption of starting materials. The excess of solvent was evaporated under reduced pressure to yield the crude solids, which were further purified by recrystallization with methanol to afford the desired title compounds (7-43).

According to the analysis of related databases, 2106-02-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Cherukupalli, Srinivasulu; Chandrasekaran, Balakumar; Kry?tof, Vladimir; Aleti, Rajeshwar Reddy; Sayyad, Nisar; Merugu, Srinivas Reddy; Kushwaha, Narva Deshwar; Karpoormath, Rajshekhar; Bioorganic Chemistry; vol. 79; (2018); p. 46 – 59;,
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Synthetic Route of 139512-70-2,Some common heterocyclic compound, 139512-70-2, name is 4-Chloro-5-fluorobenzene-1,2-diamine, molecular formula is C6H6ClFN2, 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.

Intermediate compound 5 (0.2 g, 1.24 mmol) and benzil 6d (0.26 g, 1.24 mmol) were weighed and dissolved in 20 mL glacial acetic acid. This mixture was refluxed for 2.5hr. The completion of reaction was monitored by TLC. The reaction mixture was cooled and poured into crushed ice. The precipitated product was filtered off and washed with cold water. The product was then purified by column chromatography using hexane: ethyl acetate as mobile phase. The pure fractions obtained were dried and concentrated to obtain white solids of product 7d. (yield 82%, m.p. 110-112 C). 1H NMR (400 MHz, CDCl3), delta ppm, 7.3381-7.2488 (m, 6H, Ar-3,4,5-H at C-2 and C-3), 7.441-7.411 (m, 4H, Ar-2,6-H at C-2 and C-3), 7.8824 (d, J = 9.28, -H at C-5), 8.1930 (d, J = 7.6, -H at C-8). 13C NMR (400 MHz, CDCl3), delta ppm, 113.66, 113.87, 125.44, 125.66, 128.38, 129.18, 129.27, 129.78, 129.81, 130.38, 138.38, 138.53, 138.46, 140.50, 140.61, 153.73, 153.76, 154.39, 156.93, 159.46. Mass (ESI), C20H12ClFN2, M+ and [M+2]+ peaks were found at 334 and 336, respectively.

The synthetic route of 139512-70-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Patel, Saloni B.; Patel, Bhumika D.; Pannecouque, Christophe; Bhatt, Hardik G.; European Journal of Medicinal Chemistry; vol. 117; (2016); p. 230 – 240;,
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