Tag: M.W=100-200

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 1939-99-7 as follows. Safety of Phenylmethanesulfonyl chloride

To a solution of 2-((tert-butyldimethylsilyl)oxy)ethanamine (11.7 g, 66.6 mmol) and triethylamine (11.2 mL, 79.9 mmol) in tetrahydrofuran (222 mL) at 0 C was slowly added phenylmethanesulfonyl chloride (12.7 g, 66.6 mmol) portion wise and the reaction was stirred at room temperature for 16 hours. MTBE was then added and the Et3N?HCl salt was removed byfiltration. The filtrate was then concentrated and purified by silica gel solumn chromatography (0-30% Acetone in heptane, 216 nM) to N-(2-((tert-butyldimethylsilyl)oxy)ethyl)-1- phenylmethanesulfonamide (17.8 g, 81 % yield). LCMS (ESI), mlz, 330. [M+H]+.

According to the analysis of related databases, 1939-99-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; FAUBER, Benjamin; RENE, Olivier; (86 pag.)WO2017/102796; (2017); A1;,
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Synthetic Route of 139512-70-2, A common heterocyclic compound, 139512-70-2, name is 4-Chloro-5-fluorobenzene-1,2-diamine, molecular formula is C6H6ClFN2, 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.

Example 12; 5-[(E)-2-(5-Chloro-6-fluoro- lH-benzimidazol-2-yl)-vinyl]-2-(4-methyl-imidazol- 1 -yl)-phenol trifluoroacetate salt; (E)-3-[3-Methoxy-4-(4-methyl-imidazol-l-yl)-phenyl]-acrylic acid (100 mg, 0.39 mmol) and 4-fluoro-5- chloro-benzene-l,2-diamine (62 mg, 0.39 mmol) were added to a 4-mL vial. Polyphosphoric acid (~1 ml) was added, the vial capped with a septum cap, and the reaction mixture heated to 2000C for 3h.The reaction was quenched with water and the precipitated solid collected. The residue was purified by preparative etaPLC Reverse phase (C- 18), eluting with Acetonitrile/Water + 0.05% TFA, to give the product (14 mg) as a brown solid.1H (600 MHz, dmso-d6): 2.32 (s, 3H), 7.18 (d, J= 16.4 Hz, IH), 7.30 (d, J= 1.8 Hz, IH), 7.35 (dd, J=1.7, 8.2 Hz, IH), 7.54 (d, J= 8.2 Hz, IH), 7.60 (d, J= 9.4 Hz, IH), 7.64-7.68 (m, 1 H), 7.74-7.76 (m,2H), 9.33 (s, IH).LCMS (ESI): calcd for C19H14ClFN4O [M+H]+ 369.1, found 369.1

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

Reference:
Patent; MERCK & CO., INC.; WO2008/97538; (2008); A1;,
Chloride – Wikipedia,
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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. 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, A new synthetic method of this compound is introduced below., SDS of cas: 6276-54-6

Large-Scale Synthesis of 3-Azidopropan-1-amineA solution of sodium azide (195 g, 3.0 mol) in deionized water (800 mL) was added into a three-neck round-bottom flask equipped with a condenser. Then 3-chloropropylamine hydrochloride (195 g, 1.5 mol) dissolved in 300 mL of deionized water was added. After continued stirring at 75-78 C. for 96 h, the white precipitate (NaCl) was removed as a byproduct from the reaction mixture by filtration. The yellow filtrate was basified with aqueous NaOH to pH?10-11 and further extracted with diethyl ether (5¡Á200 mL). The organic fraction was dried over anhydrous MgSO4 overnight, filtered, concentrated on a rotary evaporator, and distilled under reduced pressure to produce a colorless oil. The yield was: 108.4 g, 72%. 1H NMR (CDCl3, delta, ppm): 3.35 (t, 2H, CH2N3), 2.78 (t, 2H, NH2CH2), 1.71 (p, 2H, CH2CH2CH2), 1.27 (s, 2H, NH2).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Zhamu, Aruna; Jang, Bor Z.; US2013/5917; (2013); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

1435-48-9, name is 2,4-Dichloro-1-fluorobenzene, belongs to chlorides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C6H3Cl2F

Add to a 2 L autoclave 194 ml (2 mol) of carbon tetrachloride and 33 g (0.2 mol) of 2,4-dichlorofluorobenzene To the reactor was added 16 g of the catalyst 8 in Table 1 above, The reaction was allowed to proceed under reflux for 30 minutes, The reactor was then cooled To room temperature, To the reaction system was added 200 ml of deionized water, Reaction at 40 C for 1 hour, After completion of the reaction, a fraction of 143-144 C (35 mmHg) was collected by distillation, To give 39.1 g of a slightly yellowish liquid, Yield 86.0%

The synthetic route of 1435-48-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang Yongtai Technology Co ., Ltd; Li, yijun; Zhang, xing; Zhou, rixi; (12 pag.)CN104649890; (2016); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 39226-95-4, 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. 39226-95-4, name is 2,3-Dichlorobenzylamine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 20: Preparation of N-(4,5-dihydrothiazol-2-yl)-N-[1-(2,3-dichlorophenyl)-3- methylbut-3-enyl]amine20.1 Preparation of N-(2,3-dichlorobenzyl)-N-(4,5-dihydrothiazol-2-yl)amineA solution of 2-chloroethyl isothiocyanate (3.45 g) in diethyl ether (20 ml) was added dropwise to a solution of 2,3-dichlorobenzylamine (5.00 g) in diethyl ether(80 ml) at 0 0C and the mixture was allowed to warm up to room temperature over 3 h. An aqueous solution of sodium hydroxide (1 M, 100 ml) was then added and the mixure was further stirred for 1 h. After seperation of the phases, the organic phase was washed with water, dried over sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography to yieldN-(2,3-dichlorobenzyl)-N-(4,5-dihydrothiazol-2-yl)amine.

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, 2,3-Dichlorobenzylamine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BASF SE; WO2009/115491; (2009); 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. 821-10-3, name is 1,4-Dichlorobut-2-yne, A new synthetic method of this compound is introduced below., SDS of cas: 821-10-3

[0038] The 1 ,4-dichloro-2-butyne 14 of Example 2 is de-halogenated by base promoted elimination of HC1 to produce diacetylene 15. A mixture of 4 M aqueous potassium hydroxide (3 equivalents) and dimethyl sulfoxide (1 mL per 16 mmol potassium hydroxide) is heated to about 70-75 C. 1 ,4-dichloro-2-butyne (1 equivalent) is added slowly to the mixture while bubbling argon through the solution. The volatile product is directed through a series of two gas washing bottles containing dilute aqueous potassium hydroxide followed by two calcium chloride drying tubes and into a vessel containing anhydrous tetrahydrofuran cooled in an ice-calcium chloride bath to yield a tetrahydrofuran solution of diacetylene 15.

The synthetic route of 821-10-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EMPIRE TECHNOLOGY DEVELOPMENT LLC; KLEIN, Josef Peter; WO2015/60862; (2015); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 118-69-4, 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. 118-69-4, name is 2,6-Dichlorotoluene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To a round bottom flask was added 100 g of 2,6-dichlorotoluene, 0.5 g antimony trichloride, 59.6 g of chlorine gas was introduced at 25 C under atmospheric pressure, the reaction temperature was controlled at 25 to 30 C, Chlorine speed of 10g / h, After about 6 hours, the reaction of 2,6-dichlorotoluene was terminated by GC, and chlorine was stopped. 124.1 g of a reaction liquid was obtained, which comprised 85.4% of 2,3,6-trichlorotoluene, 1.9% of 2,4,6-trichlorotoluene, 12.7% of tetrachlorotoluene and impurities. The reaction solution was subjected to distillation to obtain 104.7 g of 2,3,6-trichlorotoluene in a yield of 86.3% GC area content of 98%.

The synthetic route of 2,6-Dichlorotoluene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Jiangsu Lianhua Technology Co., Ltd.; Lianhua Technology (Yancheng) Co., Ltd.; Fan, Xiaobin; Lin, Xingjun; Xu, Xiaoming; Huang, Chao; Chen, Donghua; Zhou, Shuyong; (8 pag.)CN105601466; (2016); A;,
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Synthetic Route of 452-73-3, A common heterocyclic compound, 452-73-3, name is 2-Chloro-4-fluoro-1-methylbenzene, molecular formula is C7H6ClF, 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.

Step A Synthesis of 2-chloro-4-fluorobenzal bromide In a flask were placed 150 g (1.04 moles) of 2-chloro-4-fluorotoluene, 391 g (2.20 moles) of N-bromosuccinimide, 3 g (0.012 mole) of benzoyl peroxide, and 800 ml of carbon tetrachloride. This mixture was refluxed overnight and then filtered. The solvent was evaporated under reduced pressure, leaving a residue of impure 2-chloro-4-fluorobenzal bromide weighing 340 g.

The synthetic route of 452-73-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; FMC Corporation; US4846875; (1989); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 95-51-2, name is 2-Chloroaniline, 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 95-51-2, Safety of 2-Chloroaniline

General procedure: Into a pressure microreactor of stainless steel of 17 mL capacity or into a glass ampule (20 mL) (results of the parallel runs were virtually identic) was charged 5-10 wt % of catalyst (0.94HY-BS, NaY-BS, 0.72KNaX-BS), 100 mmol of aniline or its derivative, and 400 mmol of dimethyl carbonate. The reactor was hermetically closed (the ampule was sealed), and was heated for 1-4 h at 150 C. After the end of the run the reactor was cooled to room temperature, opened, the reaction mixture was filtered through a bed of Al2O3. Dimethyl carbonate was distilled off, the residue was distilled at atmospheric pressure or in a vacuum, or crystallized from ethanol.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Chloroaniline, and friends who are interested can also refer to it.

Reference:
Article; Khusnutdinov; Shchadneva; Mayakova, Yu. Yu.; Ardieva; Khazipova; Kutepov; Russian Journal of Organic Chemistry; vol. 52; 11; (2016); p. 1565 – 1570; Zh. Org. Khim.; vol. 52; 11; (2016); p. 1574 – 1578,5;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 14752-66-0, 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. 14752-66-0, name is Sodium 4-chlorobenzenesulfinate belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of sodium arylsulfinates (1.0 mmol), nitroarenes (0.5 mmol), NaHSO3 (1.0 mmol), MIL-101(Fe) (10 mg, 8 mol% of Fe) in H2O (2 mL) were stirred at 60 oC for 20 h in a sealed tube. After cooling to room temperature, the aqueous solution was extracted with ethyl acetate (3 ¡Á 3 mL), and the combined extract was dried with anhydrous Na2SO4. The solvent was removed, and the crude product was separated by a flash chromatography on a silica gel column to afford the pure product 3.

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, Sodium 4-chlorobenzenesulfinate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Li, Xinxin; Chen, Fei; Lu, Guo-Ping; Tetrahedron Letters; vol. 59; 48; (2018); p. 4226 – 4230;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics