Month: August 2021

Related Products of 102-49-8, 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. 102-49-8, name is 3,4-Dichlorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: 2,2,2-Trichloro-1-(1H-pyrrol-2-yl)ethanone (2) (0.200 g, 0.94 mmol) and benzylamine (0.101 g, 0.11 mL, 0.94 mmol) were dissolved in acetonitrile (15.0 mL). Triethylamine (5 equiv, 0.65 mL) was added to the solution, and the reaction mixture stirred at 60 °C for 24 h. Solvent was removed from the reaction by rotary evaporation. The resulting yellow oil was purified using 5percent MeOH/CH2Cl2 to afford N-benzyl-1H-pyrrole-2-carboxamide (0.123 g, 65percent) as a white solid, mp 128?130 °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, 3,4-Dichlorobenzylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Dyson, Lauren; Wright, Anthony D.; Young, Kelly A.; Sakoff, Jennette A.; McCluskey, Adam; Bioorganic and Medicinal Chemistry; vol. 22; 5; (2014); p. 1690 – 1699;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 13745-86-3, 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. 13745-86-3, name is 11-Chlorodibenzo[b,f][1,4]thiazepine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 2Preparation of 11-piperazinyl-Dibenzo[B,F][1,4]Thiazepine,DihydrochlorideDimethylsulfoxide (3.0 L); piperazine (2.45 Kg); toluene (3.0 L) were charged at room temperature under nitrogen and the mixture was heated to 50 C. to 60 C.; stirred at 50 C. to 60 C. till solid dissolves and cooled to 25 C. to 30 C. To it a solution of 11-chloro-dibenzo[b,f]1,4]thiazepine (1.0 Kg) in toluene (6.0 L) was charged at 25 C. to 30 C. and stirred for 3 hours at 25 C. to 30 C. and monitored to completion. The reaction mixture was charged slowly into DI water (45 L) at 25 C. to 30 C. and stirred for 30 minutes at 25 C. to 30 C. The layers were separated at room temperature and the organic layer was washed with DI water (3×3.0 L) at room temperature. The solvent was recovered from the organic layer under vacuum at 50 C. to 55 C. to obtain oil. Ethanol (5 L) was charged into the residue and stirred to dissolve at room temperature. Concentrated hydrochloric acid (0.72 L) was added slowly at 25 C. to 30 C. and stirred until the solid precipitated. The mixture was stirred for 10 hours at 25 C. to 30 C. after precipitation, cooled to 0 C. to 5 C. and stirred for 1 hour at 0 C. to 5 C. The solid was filtered and washed with ethanol (1 L) at 0 C. to 5 C. The solid was added to pre-cooled ethanol (5 L) at 0 C. to 5 C. and stirred for 15 minutes at 0 C. to 5 C. The solid was filtered at 0 C. to 5 C. and washed with ethanol (1 L) at 0 C. to 5 C. The wet cake was unloaded at room temperature under nitrogen atmosphere and dried under vacuum at 55 C. to 60 C. until the moisture content is NMT 5.0% to obtain the title compound.Yield: 1.10 Kg

The synthetic route of 11-Chlorodibenzo[b,f][1,4]thiazepine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; RANBAXY LABORATORIES LIMITED; US2012/71649; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

These common heterocyclic compound, 622-86-6, name is (2-Chloroethoxy)benzene, 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. Computed Properties of C8H9ClO

2-(4-Fluorophenyl)butanoic acid (250.3 mg, 1.4mmol) was suspended with stirring in trifluoroacetic anhydride (194.2 uL, 2.0mmol). Then (2-chloroethoxy)benzene (173 uL, 1.3 mmol) was added the resultingmixture was stirred at room temperature overnight. The reaction was quenchedwith saturated sodium bicarbonate solution (5 mL) and extracted with ethylacetate (2 x 15 mL). The combinedorganic layers were dried over anhydrous magnesium sulfate and concentrated ona rotary evaporator. The resultingresidue was purified by reverse-phased chromatography (C-10 column, gradient ofacetonitrile in water with 0.1% trifluoroacetic acid) to afford 105.2 mg (26%)of the desired product as a yellow solid.1H NMR (400 MHz, CDCl3) delta 7.90 (d, J=8.8 Hz, 2H), 7.50 (d,J=8.7 Hz, 2H), 7.23 (m, 2H), 6.95 (d, J=8.7 Hz, 2H), 4.25 (m, 3H), 3.86 (t,J=7.2 Hz, 2H), 2.18 (m, 1H), 1.60 (m, 1H), 0.90 (t, J=7.3 Hz, 3H); MS (ESI)(m/z) 321.1/323.1 (M+H)+.

The synthetic route of (2-Chloroethoxy)benzene 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

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. 3386-33-2, name is 1-Chlorooctadecane, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C18H37Cl

EXAMPLE 1 Preparation of a compound of formula (I) in which R1 is a stearyl radical, R2 is a hydroxypropyl radical, n=6.3 and p=14 52.5 g (173 mmol) of stearyl chloride were added dropwise for 20 minutes at 20 C. to a solution of 12.4 g (8.3 mmol) of hydroxypropyl-beta-cyclodextrin (n=6.3), sold by the company Aldrich, in 100 ml of anhydrous pyridine. After 5 hours’ stirring at ambient temperature, the reaction mixture was poured into 400 ml of ethanol. The solid obtained was filtered off and washed three times with 200 ml portions of hot ethanol. After drying, 40.5 g of a light-beige solid which had a melting point of 39 C. were obtained. Infrared: ester band at 1745 cm-1

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 3386-33-2.

Reference:
Patent; L’Oreal; US5854225; (1998); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 7051-16-3, name is 1-Chloro-3,5-dimethoxybenzene, 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 7051-16-3, Computed Properties of C8H9ClO2

General procedure: Under argon protection, NiCl2 · 6H2O (0.05mmo 1,11.9mg), dppf (0.06mmol, 33.3mg), Zn (0 · 2mmol, 13.0mg), DMAP (1.0mmol, 122.2mg), Zn (CN) 2 (0.8mmol) , 93.9mg),p-Chloroanisole (1.0 mmol, 140.6 mg) and acetonitrile (5.0 mL) were sequentially added in a 25.0 mL sealed tube, then directly put it into the oil bath at 60 C, and heating was stopped after 6h, and cooled to room temperature, the reaction solution was directly filtered through a short silica gel column, washed with dichloromethane, concentrated and purified by silica gel column chromatography( given that the product is most easily pulled out, in order to avoid loss of sample mix, unless otherwise noted, both are wet method). Eluent: petroleum ether / ethyl acetate = 20:1, the product was 117.2 mg as a white solid, yield 88%, and 1H NMR purity was greater than 98%.

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-Chloro-3,5-dimethoxybenzene, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chinese Academy Of Sciences Shanghai Organic Chemistry Institute; Liu Yuanhong; Zhang Xingjie; (34 pag.)CN108623495; (2018); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 14752-66-0,Some common heterocyclic compound, 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, molecular formula is C6H4ClNaO2S, 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.

Description 3 3-[(4-Chlorophenyl)sulfonyl]-8-fluoroquinoline (D3) EPO A mixture of 8-fluoro-3-iodoquinoline (D1 ) (750 mg, 2.75 mmol), sodium 4- chlorobenzenesulfinate (1.1 g, 5.5 mmol), copper (I) iodide ( 52 mg, 0.275 mmol) and potassium carbonate (380 mg, 2.75 mmol) was treated with lambda/./V-di methyl- 1 ,2- ethanediamine (49 mg, 0.55 mmol) and anhydrous dimethylsulphoxide (4 ml). The mixture was stirred at 1000C under argon for 8 hr, and cooled to 200C. The reaction mixture was diluted with water (60 ml) and extracted with ethyl acetate (3 x 40 ml). The organic extracts were combined, washed with water (60 ml) and brine (60 ml), dried over magnesium sulphate, and evaporated to dryness. The residue was dissolved in a 1 :1 mixture of dimethylsulphoxide and acetonitrile and purified by mass-directed auto- preparative chromatography using 10 minute gradients containing water and between 50% and 99% acetonitrile with 0.1% formic acid. Product fractions were collected and evaporated to yield the title compound as a white solid (295 mg, 33%). deltaH (CDCI3, 400MHz) 7.51-7.69 (4H, m), 7.79 (1 H, d, J = 8 Hz), 7.96-7.99 (2H, m), 8.84 (1 H, d, J = 2 Hz), 9.30 (1 H, d, J = 2 Hz) Mass spectrum: C15H9CIFNO2S requires 321 ; found 322 (MH+)

The synthetic route of 14752-66-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXO GROUP LIMITED; WO2007/39220; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 15205-11-5, name is 2-Chloro-4-fluorobenzylamine, molecular formula is C7H7ClFN, 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: C7H7ClFN

3-Methyl-5-(2-methylpropyl)-1 /-/-pyrazol-4-yl]acetic acid (0.170 g, 0.43 mmol, prepared as described below) was dissolved in a mixture of dimethylformamide (1 ml) and dichloromethane (3 ml) and and to this was added water soluble carbodiimide (0.099 g, 0.52 mmol), 1-hydroxybenzotriazole (0.070 g, 0.52 mmol), and N-ethyl morpholine (0.164 ml, 1.29 mmol). The mixture was stirred for 10 minutes and then [(2-chloro-4-fluorophenyl)methyl]amine (0.082 g, 0.52 mmol) was added. The mixture was stirred overnight at room temperature and then saturated aqueous sodium hydrogen carbonate (2 ml) was added to the mixture. After stirring for a further 10 minutes the organic phase was separated by filtration through a hydrophobic frit. The aqueous layer was washed with a further aliquot of dichloromethane (2-3 ml) and the organic phase was again separated and then the combined organic phases were evaporated to give the crude product as a yellow oil. The crude material was purified by mass-directed automated HPLC to give the pure product as a white solid after freeze-drying of the collected product fractions (0.080 g)-LC/MS [M+H]+ = 338 retention time = 2.32 minutes.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 15205-11-5, its application will become more common.

Reference:
Patent; GLAXO GROUP LIMITED; WO2007/141267; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference 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.

To a mixture of 4-chioroanisole (62 iL, 0.50 mmol, I equiv), 1-napthylboronic acid (94 mg, 0.55 mmol, 1.1 equiv), and K3P04H20 (0.35 g, 1.5 mmol, 3 equiv) was added toluene (800a THF stock solution of 3 and PAd3 (100 pL, 0.25 .tmol Pd/PAd3) and the mixture was stirred at room temperature for 5 h. The reaction mixture was diluted with ethyl acetate then extracted with water. The combined organic layers were evaporated and the crude product waspurified by flash chromatography. After drying, 104 mg of 6 (89 %) was obtained as a white solid. NMR spectroscopic data agreed with literature values.

The synthetic route of 623-12-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THE TRUSTEES OF PRINCETON UNIVERSITY; CARROW, Brad P.; CHEN, Liye; (51 pag.)WO2017/75581; (2017); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 13726-14-2, name is 4-Chloro-3-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 13726-14-2, Quality Control of 4-Chloro-3-methoxyaniline

General procedure: The mixture of aniline 1 (1.2 mmol), alcohol (0.4 mmol), and ReH7(PCy3)2 (10 mol %,18 mg) were added into the flask. Then, anisole (0.5 mL) was added. The flask was evacuated and backfilled with CO (1.5 atm). The reaction mixture was vigorously stirred at 150 oC under for 20-36 h. After the reaction finished, the reaction mixture was cooled to room temperature and extracted with ethyl acetate (3 × 5 mL), the combined organic phases were dried over anhydrous Na2SO4 and the solvent was evaporated under vacuum. After removing the solvents in vacuum, the residue was purified by flash column chromatography on silica gel or preparative TLC on GF254to afford the desired amination products.

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:
Article; Abdukader, Ablimit; Jin, Hongming; Cheng, Yixiang; Zhu, Chengjian; Tetrahedron Letters; vol. 55; 30; (2014); p. 4172 – 4174;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 60811-21-4,Some common heterocyclic compound, 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, molecular formula is C6H3BrClF, 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 21 6-(3-Chloro-4-fluoro-phenyl)-4-isopropyl-3,4-dihydro-1H-quinoxalin-2-one A mixture of (3,4-dihydro-4-isopropyl-2-oxoquinoxalin-6-yl)boronic acid (2.4 g, 10 mmol), 4-bromo-2-chlorofluorobenzene (2 g, 10 mmol), potassium carbonate (4 g, 30 mmol), and tetrakis(triphenylphosphine)palladium(0) (0.46 g, 0.4 mmol) in dimethoxyethane (100 ml), ethanol (25 ml) and water (25 mol) was heated to reflux for 6 hrs. After cooling to room temperature the mixture was diluted with water and extracted with ethyl acetate (3*). The combined organic layers were washed with water, then brine, dried (MgSO4) and evaporated to obtain crude product (2.9 g, 91%). Recrystallization from EtOAc/hexane afforded the title compound, mp 208-213 C.: 1H-NMR (DMSO-d6) delta1.16 (d, J=6.59 Hz, 6H), 3.56 (s, 2H), 4.22 (septet, J=6.59 Hz, 1H), 6.86 (d, J=7.91 Hz, 1H), 6.96 (dd, J=7.91, 1.76 Hz, 1H), 7.01 (d, J=1.76 Hz, 1H), 7.43 (t, J=9.01 Hz, 1H), 7.61 (m, 1H), 7.82 (dd, J=7.14, 2.31 Hz, 1H), 10.47 (s, 1H). MS (EI) m/z 318 [M]++1 chlorine.

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

Reference:
Patent; American Home Products Corporation; Ligand Pharmaceuticals, Inc.; US6380235; (2002); B1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics