Tag: M.W=100-200

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);,
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Electric Literature of 83121-15-7, 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. 83121-15-7, name is 3,5-Dichloro-2,4-difluoroaniline belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2.7 mmol of 2,4-difluoro-3,5-dichloro-aniline, and 20 ml of 1,2-dichloroethane in a 100 ml round bottom flask and stirred until the 2,4-difluoro-3,5diclofenac was completely dissolved, was added dropwise with stirring 3 mmol of 4-methyl-1,2,3-thiadiazole-5-formylphenyl isocyanate, dropwise over 15 minutes immediatelythereafter precipitation, followed by stirring at room temperature for 8 hours aftercompletion of the reaction, allowed to stand, the solid product was suction filtered,the filtrate solvent was removed by rotary evaporation, ethyl acetate with a volumeratio of 1:3: recrystallized from petroleum ether after the refrigerator to precipitatea solid, the solid product was combined with 1:3 volume ratio of ethyl acetate:petroleum ether, washed and dried to obtain the product; mp: 187-189 C, yield 92%;

The synthetic route of 3,5-Dichloro-2,4-difluoroaniline has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Lier Chemical co Limited; Nankai University; Fan, ZhiJin; Guo, dandan; fan, Qian; Yang, Wei Qing; Fu, yifeng; Zhao, Hui; Wang, Shouxin; Wang, huan; Mi, Na; (37 pag.)CN102225918; (2016); B;,
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Adding a certain compound to certain chemical reactions, such as: 6276-54-6, name is 3-Chloropropan-1-amine 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 6276-54-6, Quality Control of 3-Chloropropan-1-amine hydrochloride

Step 1: Synthesis of 1-azido-3-aminopropane 1 Synthesis is carried out according to the following reaction scheme: This compound was obtained according to a synthesis previously described by Carboni, B. et al. (Macromolecules, Vol. 40, No. 16, 2007/Carboni, B.; Benanlil, A.: Vaultier, M. J. Org. Chem. 1993, 58, 3736). An aqueous solution (30 mL) of 3-chloropropylamine hydrochloride (4 g; 30.8 mmol) and of sodium nitride (6 g; 92.3 mmol, 3 equiv) is heated at 80 C. for 17 h. After evaporation of the water, the reaction mixture is put in an ice bath. 50 mL of diethyl ether and 4 g of potassium hydroxide are added. The phases are separated. The product is extracted from the aqueous phase with 2*20 ml, of diethyl ether. The organic phase is then dried over magnesium sulfate and filtered. After evaporation, the oil obtained is purified by distillation at reduced pressure. (2.46 g; yield: 80%; colorless oil) 1H NMR (300 MHz, CDCl3), delta (ppm): 3.33 (t, 2H, CH2N3); 2.55 (t, 2H, Cl2NH2); 2.34 (s, 2H, NH2); 1.55 (q, 2H, CH2CH2CH2). FT-IR (ATR, cm-1): 2100 (N3)

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; Centre National de la Recherche Scientifique; Coudane, Jean; Darcos, Vincent; El Habnouni, Sarah; Garric, Xavier; Lemaire, Laurent; Nottelet, Benjamin; US2014/302324; (2014); A1;,
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Electric Literature of 13078-80-3, 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. 13078-80-3, name is 2-(2-Chlorophenyl)ethanamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Propyl N-cyano-6-amino-3-pyridinecarboximidate (200 mg, 0.98 mmol) and 2-(2-chlorophenyl)ethylamine (170 mg, 1.09 mmol) were dissolved in a mixture of methanol (10 ml) and DMF (1.5 ml), and the mixture was stirred at room temperature for 2.5 hours. The reaction mixture was concentrated under reduced pressure and subjected to silica gel column chromatography (Wako Gel C-200, 25 g), and elution was conducted with chloroform:methanol (30:1) to give the title compound (250 mg, yield 85%) as colorless powder. Mp 222 C. IR (KBr) cm-1:3220, 2160, 1570, 740. 1 H-NMR (90 MHz, DMSO): delta (ppm) 8.91(1Hr brs, NH), 8.13(1H, d, J=2.5Hz, H-6), 7.60(1H, dd, J=2.5, 8.6Hz, H-4), 7.45-7.2(4H, C6 H4 Cl), 6.60(2H, brs, NH2), 6.48(1H, d, J=8.6Hz, H-3), 3.56(2H, m, NHCH2 CH2 C6 H4 Cl), 3.02(2H, t, J=7.0Hz, NHCH2 CH2 C6 H4 Cl).

The synthetic route of 2-(2-Chlorophenyl)ethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Kirin Beer Kabushiki Kaisha; US5508293; (1996); A;,
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Some common heterocyclic compound, 13726-14-2, name is 4-Chloro-3-methoxyaniline, molecular formula is C7H8ClNO, 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. Product Details of 13726-14-2

Benzoyl isothiocyanate (8.8 mL, 64 mmol) was added dropwise to a solution of 4-chloro- 3-methoxy-benzenamine (10 g, 63 mmol) in 160 mL THF. The mixture was stirred at room temperature for 40 minutes, volatiles were removed and the residue was dissolved in 400 mL methanol. A solution of potassium carbonate (26.3 g, 190 mmol) in 200 mL water was added and the mixture was stirred at room temperature for 90 minutes. The title product (13.5 g, 98%) precipitated after removal of 450 mL of the solvents. MS (m/e): 216.0, 218.0 (M+)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 13726-14-2, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2005/58887; (2005); A1;,
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Application of 918538-05-3, 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. 918538-05-3, name is 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of 2,4-dichloropyrrolo[1,2-f][1,2,4]triazine (4a) (0.5 g, 2.7 mmol) in 2-Propanol (6 mL) was added (S)-pyrrolidin-2-ylmethanol (0.39 mL, 4.0 mmol), DIPEA (1.39 mL, 8.0 mmol) and heated at 90 C for 1 hr. The reaction was cooled to room temperature and solid obtained was collected by filtration to afford (S)-(l-(2-chloropyrrolo[2,l-f][l,2,4]triazin-4- yl)pyrrolidin-2-yl)methanol (96a) (0.49 g, 73 % yield) as a white solid; NMR (300 MHz, DMSO-i/e): delta 7.70 (dd, J= 2.6, 1.4 Hz, 1H), 6.97 (dd, J= 4.7, 1.6 Hz, 1H), 6.80 – 6.57 (m, 1H), 5.15 (t, J = 5.7 Hz, 1H, D2O exchangeable), 4.87 (t, J= 5.7 Hz, 1H), 4.44 (d, J= 17.8 Hz, 1H), 4.05 – 3.82 (m, 1H), 3.72 – 3.39 (m, 2H), 2.22 – 1.84 (m, 4H). MS (ES+): 253.3, 255.3 (M+2); MS (ES-): 287.2, 289.2 (M+Cl).

The chemical industry reduces the impact on the environment during synthesis 2,4-Dichloropyrrolo[2,1-f][1,2,4]triazine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; BIOCRYST PHARMACEUTICALS, INC.; KOTIAN, Pravin, L.; BABU, Yarlagadda, S.; KUMAR, V., Satish; ZHANG, Weihe; LU, Peng-Cheng; RAMAN, Krishnan; (747 pag.)WO2018/232094; (2018); A1;,
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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 3260-88-6 as follows. Recommanded Product: 3260-88-6

Reference Example 44 2-Chloro-6-methoxybenzyl bromide A mixture of 3-chloro-2-methylanisole (2 g), N-bromosuccinimide (2.39 g) and 2,2′-azobis(2-methylpropionitrile) (32 mg) in carbon tetrachloride (15 mL) was heated at reflux for 3 hours. The insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane – n-hexane/ethyl acetate = 4/1) to give the title compound (2.9 g).

According to the analysis of related databases, 3260-88-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Kissei Pharmaceutical Co., Ltd.; EP2143724; (2010); A1;,
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Application of 870-24-6, 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. 870-24-6, name is 2-Chloroethanamine hydrochloride belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

2-Chloroethanamine hydrochloride (4.6 g, 40 mmol), NEt3 (18 mL, 132 mmol) And 50 mL of methylene chloride. The reaction was stirred at room temperature and trimethylchlorosilane (90 mmol, 9.8 g, 11.4 mL) in dichloromethane (20 mL) was added to the system. The reaction was stirred at room temperature overnight. After the reaction was completed, excess triethylamine, trimethylchlorosilane and methylene chloride were removed under reduced pressure. To the resulting residue was added 60 mL of n-hexane. The reaction was stirred at room temperature for 30 minutes and filtered to remove NEt3.HCl. After the filtrate is concentrated, The target product was obtained by distillation under reduced pressure (6.0 g, 68%).

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

Reference:
Patent; Tsinghua University; Liu Qiang; Fu Shaomin; Shao Zhihui; Wang Yujie; (20 pag.)CN107445995; (2017); A;,
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Adding a certain compound to certain chemical reactions, such as: 3843-97-8, name is 5-Chloro-2-ethylaniline, 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 3843-97-8, Quality Control of 5-Chloro-2-ethylaniline

A mixture of 5-chloro-2-ethylaniline (3.35 g, 21.5 mmol), p-toluensulfonic acid (12.29 g, 64.6 mmol) and water (2.15 mL) were ground in a mortar for few minutes, to obtain a homogeneous paste to which solid sodium nitrite (3.71 g, 53.8 mmol) was added and the paste ground for 10 min. Solid potassium iodide (8.94 g, 53.8 mmol) was added and the paste ground for 20 min. The paste was then dissolved in water (50 mL) and treated with sodium sulfite (10% aq. sol.), before being extracted with EtOAc (3 x 100 mL). The combined organic layers were dried over sodium sulfate and the crude was purified by flash chromatography (hexane) to obtain the title compound as a light-yellow oil (4.35 g, 76%).1H NMR (400 MHz, DMSO-d6) delta ppm 1.12 (t, J=7.51 Hz, 3 H), 2.66 (q, J=7.53 Hz, 2 H), 7.29 – 7.35 (m, 1 H), 7.42 (dd, J=8.30, 2.20 Hz, 1 H), 7.87 (d, J=2.20 Hz, 1 H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; NERVIANO MEDICAL SCIENCES S.R.L.; BRASCA, Maria, Gabriella; BERTRAND, Jay, Aaron; GNOCCHI, Paola; MOTTO, Ilaria; NESI, Marcella; PANZERI, Achille; VIANELLO, Paola; WO2013/14039; (2013); A1;,
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Reference of 87851-77-2, 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. 87851-77-2, name is O-(3-Chloroallyl)hydroxylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The cyclohexanone derivatization method is described immediately below. Weigh about 2.00 g of sample in a vial containing 2.20 g of cyclohexanone; Add 50percent sodium hydroxide if necessary to bring pH to above 9. Stir the mixture in the capped vial at 50° C. for 2 hours. After cooling, add 8.0 g of dichloromethane and shake for one minute. Settle the mixture for 5 minutes. Take the organic phase for gas chromatographic (GC) analysis. CPHA purity and impurity profile are directly based on GC area. Hydroxylamine content is calculated based on the integration area of cyclohexanone oxime (cyclohexanoxime) peak and O-(chloro-2-propenyl)cyclohexanoxime peak.

The synthetic route of O-(3-Chloroallyl)hydroxylamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Honeywell Corporation; US2005/85645; (2005); A1;,
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