Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 6940-78-9, name is 1-Bromo-4-chlorobutane, 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 6940-78-9, category: chlorides-buliding-blocks

Example 7 Preparation of 7-CBQ by reaction of 7-HQ with 1-bromo-4-chlorobutane in 2-propanol in Presence of About 85% Solid potassium hydroxide A mixture of 7-HQ (40 g, 0.245 mole), 1-bromo-4-chlorobutane (85.7 ml, 127.5 g, 0.735 mole, 3 eq.) and 85% solid potassium hydroxide (21 g, 0.318 mole, 1.3 eq.) in 2-propanol (200 ml) was heated under reflux for 2 hours. The hot reaction mixture was filtered and the solvent and excess 1-bromo-4-chlorobutane were removed to dryness in vacuum. 2-Propanol (125 ml) was added to the residue thus obtained and the mixture was heated under reflux to obtain a solution. A solution of 47% aqueous sodium hydroxide solution was added to the hot solution to produce a pH of about 10-11 and the mixture was set aside at 10-15 C. for 6 hours. A colorless precipitate was collected by filtration, washed with the cold mixture of water and 2-propanol (1:3, 50 ml) and water (100 ml) and dried under reduced pressure at 50 C. overnight to obtain 7-(4-chlorobutoxy)-3,4-dihydro-2(1H)-quinolinone (56.8 g) in 91.3% yield, having a purity of 98.5% (by HPLC). Re-crystallization from acetone gave colorless needle crystals: mp 104.0-105.5 C.

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; Naddaka, Vladimir; Brand, Michael; Davidi, Guy; Klopfer, Eyal; Gribun, Irina; Arad, Oded; Kaspi, Joseph; US2006/79689; (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. 2106-04-9, name is 3-Chloro-2-fluoroaniline, A new synthetic method of this compound is introduced below., Computed Properties of C6H5ClFN

6-Acetoxy-4-chloro-7-methoxyquinazoline (prepared as described in Example 25- 5 of in WO01/66099, 6.00 g, 23. 8 mmol) and 3-chloro-2-fluoroaniline (3.46 g, 23. 8 mmol) were suspended in iso-propanol (200 ml). The mixture was heated to 80C under reflux for 3 hours. The solvent was evaporated; the residue was crystallised from acetonitrile, giving 6-ACETOXY-4- (3-CHLORO-2-FLUOROANILINO)-7-METHOXYQUINAZOLINE hydrochloride as a pale pink crystalline solid (8.16 g, 92%) ; 1H NMR : 2.37 (s, 3H), 4. 00 (s, 3H), 7.34 (ddd, 1H), 7. 48 (s, 1H), 7.52 (ddd, 1H), 7.61 (ddd, 1H), 8. 62 (s, 1H), 8. 86 (s, 1H) ; Mass Spectrum : 362.4, 364.4.

The synthetic route of 2106-04-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENEKA UK LIMITED; WO2005/26156; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 4152-90-3, name is (3-Chlorophenyl)methanamine, 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 4152-90-3, Formula: C7H8ClN

General procedure: In a typical process, into a 25 ml autoclave equipped with a magnetic stirrer were added 5percentRu/AC (0.03 mmol, 3 molpercent), benzylamine (1 mmol), 5 mL toluene at room temperature successively. After which the resulting reaction mixture was heated at 150 °C for 4 h under 0.5 MPa of oxygen atmosphere. The final reaction conversion and selectivity towards the corresponding nitriles were determined by Gas Chromatograph. After reaction, the product was purified by column chromatography of the reaction mixture on neutral alumina using hexanes/dichloromethane (80:20) or hexanes/EtOAc (30:1) as eluent.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (3-Chlorophenyl)methanamine, and friends who are interested can also refer to it.

Reference:
Article; Niu, Baoqiang; Lu, Fei; Zhang, Hong-Yu; Zhang, Yuecheng; Zhao, Jiquan; Chemistry Letters; vol. 46; 3; (2017); p. 330 – 333;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 39885-50-2,Some common heterocyclic compound, 39885-50-2, name is 2-Chloro-4-(trifluoromethyl)aniline, molecular formula is C7H5ClF3N, 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 A mixture (301 g) of 2-chloro-4-trifluoromethylaniline, 2-chloro-5-trifluoromethylaniline and N-methylpyrrolidone (NMP) (1.06 m/m) was mixed with 500 ml chlorobenzene. Sulfuryl chloride (148.4 g) was added to the mixture at 55-60° C. over a period of 4 hours and the reaction mixture was maintained at 55-60° C. for 4 hours. Reaction medium on treatment and fractionation gave 0.84 m of 2,6-dichloro-4-trifluoromethylaniline, 95percent yield on 2-chloro-4-trifluoromethyl aniline.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-Chloro-4-(trifluoromethyl)aniline, its application will become more common.

Reference:
Patent; Gharda, Keki Hormusji; US2013/30190; (2013); 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. 39885-50-2, name is 2-Chloro-4-(trifluoromethyl)aniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 2-Chloro-4-(trifluoromethyl)aniline

General procedure: Aniline (140mg, 1.5mmol) and Et3N (202mg, 2mmol) were dissolved in 5mL of dichloromethane and slowly added dropwise to a solution of triphosgene (BTC) (223mg, 0.75mmol) in 10mL of dichloromethane at 0°C. The mixture was then stirred at 0°C for 1h. Then, 5a (300mg, 1mmol) in 1mL of DMF was added at 0°C, and the mixture was then stirred at room temperature for 30min, and the solvent was distilled with a rotary evaporator. The residue was washed with water (10mL×3) and purified via silica gel flash column chromatography to afford 1-(3-((2S,5S)-5-((1H-indol-3-yl)methyl)-3,6-dioxopiperazin-2-yl)propyl)-3-phenylurea (6a) as a pale powder in 74percent yield. Compounds 6b?v, 7a?k and 8a?k were prepared similar to 6a.

The synthetic route of 39885-50-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sun, Haiyang; Li, Hui; Wang, Jiayi; Song, Gonghua; Chinese Chemical Letters; vol. 29; 6; (2018); p. 977 – 980;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 2401-24-3, These common heterocyclic compound, 2401-24-3, name is 2-Chloro-5-methoxyaniline, 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.

6-Chloro-3-methoxyaniline (1.57 g, 10 mmol) was dissolved in ethyl acetate (15 mL)Under ice-cooling,To the above solution was added portionwise1,3-dibromo-5,5-Dimethylhydantoin(3.1 g, ll mmol),After the addition, the reaction solution was allowed to react under ice-cooling for 1 hour,The reaction solution was quenched with saturated potassium carbonate solution,The organic phase was separated,Respectively, with water,Washed with a saturated saline solution,Dried over anhydrous sodium sulfate,Filtered, concentrated under reduced pressure,Bromo-2-chloro-5-methoxyaniline(Brown solid, 1.96 g).

The synthetic route of 2401-24-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Pharmaceuticals Holding Co., Ltd.; Wan, huixin; Shen, JingKang; Li, ChunLi; Han, yanan; Liu, Haiyan; Zhou, ZhaoLi; Li, Ping; Li, Yufeng; Chen, gang; Xu, Jia; (54 pag.)CN103848785; (2016); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 29671-92-9, 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. 29671-92-9, name is Carbamimidic chloride hydrochloride, This compound has unique chemical properties. The synthetic route is as follows.

Step 3; 2-Amino-6- (2-chlorophenoxymethyl)benzonitrile mg; 0.31mmol) and chloroformamidine hydrochloride (53.0 mg, 0.46 mmol) were heated at 140 C in diglyme for 3 hours. The reaction mixture was diluted with water, stirred for 2 hours, filtered, washed with water and dried. Purification by silica gel chromatography (5% methanol in dichloromethane) yielded 50 mg of 5-(2- chlorophenoxymethyl) quinazoline-2,4-diamine.

The chemical industry reduces the impact on the environment during synthesis Carbamimidic chloride hydrochloride. I believe this compound will play a more active role in future production and life.

Reference:
Patent; DECODE CHEMISTRY, INC.; SINGH, Jasbir; GURNEY, Mark E.; WO2005/123724; (2005); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 106-39-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 106-39-8 as follows.

General procedure: In a thermostatted bath at 25C (or 60C for compounds 18 and 28), a 25 mL Schlenk flask was charged in air with a magnetic stir bar, arylbromide (0.5 mmol), arylboronic acid (0.6 mmol), K2CO3 (0.6 mmol), 1 (26.6 mg, 1mol-%), ethanol (1.5 mL), and water (0.5 mL). The reaction mixture was kept under vigorous stirring until the GC control showed no residual aryl bromide in solution. Water (10 mL) was added to the suspension and the organics were extracted with dichloromethane (3×10 mL). The solution was dried over Na2SO4 and then passed through a column filled with silica gel (diatomaceous earths were used in the case of compound 28). Elimination of the solvent under vacuum gave the desired biaryl as white microcrystalline solid. Purity (96÷99%) was established by GC and 1H NMR. 1H and 13C{1H} NMR data of compounds 8-28. Spin multiplicity is given by s=singlet, br s=broad singlet, q=quartet, st=septet, qq=quartet of quartets, ddd=doublet of doublets of doublets, m=unresolved multiplet. 4-Chloro-4′-methoxy-1,1′-biphenyl (17). Yield 94%. C13H11OCl (218.68): calcd. C 71.40, H 5.07; found C 71.27, H 5.13. 1H NMR (CDCl3): delta = 7.58-7.44 (4H, m), 7.42-7.33 (2H, m), 7.08-6.95 (2H, m), 3.86 (3H, s, OCH3) ppm. 13C NMR (CDCl3): delta = 159.3, 139.2, 132.6, 132.4, 128.8, 128.0, 127.9, 114.3, 55.3 (OCH3) ppm.

According to the analysis of related databases, 106-39-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Del Zotto, Alessandro; Colussi, Sara; Trovarelli, Alessandro; Inorganica Chimica Acta; vol. 470; (2018); p. 275 – 283;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 2533-69-9, The chemical industry reduces the impact on the environment during synthesis 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate, I believe this compound will play a more active role in future production and life.

General procedure: Preparation of 2-methyl-6-nitro-2H-indazole (5d). To a stirred mixture of 6-nitro-1H-indazole (1.0 g, 0.0061 mmol) in dichloromethane (25.0 mL) was added trifluoromethanesulfonic acid (0.54 mL, 0.0061 mmol), stirred for 5-10 min at 25-35 C. To this mixture was added methyl 2,2,2,-trichlroacetimidate (2.69 g, 0.015 mmol) at room temperature. The reaction mixture was stirred at room temperature for 16-18 h under N2. After reaction completion, chilled saturated NaHCO3 solution was added. The aqueous and organic phases were separated. Aqueous phase was extracted with dichloromethane 10 mL. Combined organic layers were washed with DM water (2 × 10 mL). Organic layer was dried over anhydrous Na2SO4, filtered, and evaporated completely under vacuum to obtain 2-methyl-6-nitro-2H-indazole (1.03 g, 95.0%) as a yellow solid.

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, Methyl 2,2,2-trichloroacetimidate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Baddam, Sudhakar Reddy; Uday Kumar; Panasa Reddy; Bandichhor, Rakeshwar; Tetrahedron Letters; vol. 54; 13; (2013); p. 1661 – 1663;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 932-96-7, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 932-96-7 as follows.

General procedure:To a solution of 3-(chlorosulfonyl)benzoic acid (1.0 equiv, ca. 0.1 M) in dichloromethane, 4-bromo-N-methylaniline (3.1 equiv) was slowly added at 0 C with stirring. The mixture was stirred at room temp for 12 h. The solvent was removed with a nitrogen gas stream, the mixture was treated with 1 M NaOH (> 10 equiv), and was extracted with ether three times. The aqueous fraction was then acidified with 3 M HCl to pH ~1. The mixture turned cloudy during the addition. The resulting precipitate was collected by suction filtration on a Buchner funnel, washed with distilled water, and dried overnight at reduced pressure to give 3-(N-(4-bromophenyl)-N-methylsulfamoyl)benzoic acid (7a, 50-60%), which was used without further purification. To a solution of 7a (1.0 equiv, ca. 0.1 M), was added 4-chloro-N-methylaniline (1.1 equiv), EDCI (1.3 equiv), and DMAP (0.1 equiv). The mixture was stirred at room temp for 12 h and then diluted with excess EtOAc. The organic mixture was washed with 1 M aqueous HCl (2 times), 1 M aqueous NaHCO3 (2 times), and brine. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo to yield a crude product, which was purified by silica gel column chromatography to give 3a as a thick gel.

According to the analysis of related databases, 932-96-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Choi, Soo Hyuk; Quinti, Luisa; Kazantsev, Aleksey G.; Silverman, Richard B.; Bioorganic and Medicinal Chemistry Letters; vol. 22; 8; (2012); p. 2789 – 2793;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics