Tag: M.W=100-200

Some common heterocyclic compound, 2687-12-9, name is Cinnamyl chloride, molecular formula is C9H9Cl, 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: C9H9Cl

General procedure: A representative procedure of skeleton 4 is as follows: K2CO3 (400 mg, 2.9 mmol) was added to a solution of 3 (1.0 mmol) in acetone (10 mL) at rt. The reaction mixture was stirred at rt for 10 min. Cinnamyl chloride (1.05 mmol) was added to the reaction mixture at rt. The reaction mixture was stirred at reflux for 8 h. The reaction mixture was cooled to rt, concentrated, and extracted with CH2Cl2 (3¡Á20 mL). The combined organic layers were washed with brine, dried, filtered, and evaporated to afford crude product under reduced pressure. Purification on silica gel (hexanes/EtOAc=6:1 to 1:1) afforded 4.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2687-12-9, its application will become more common.

Reference:
Article; Chang, Meng-Yang; Lu, Yi-Ju; Cheng, Yu-Chieh; Tetrahedron; vol. 71; 8; (2015); p. 1192 – 1201;,
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Related Products of 626-43-7, These common heterocyclic compound, 626-43-7, name is 3,5-Dichloroaniline, 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.

3,5-dichloroaniline 20 g (0.32 mol) was dissolved in CH2Cl2 (150 mL) and sat. aq. NaHCO3 (50 mL) was added. The resulting biphasic solution was cooled to 0 C. and thiophosgene (0.38 mol) was then carefully added via syringe. After the addition was completed, the reaction was allowed to warm to room temperature and stirred for 2 h. The organic layer was separated and dried over Na2SO4. The filtrate was concentrated under reduced pressure to afford title compound 47.1 g as a yellow oil, yield: 72.1%.

The synthetic route of 626-43-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shenyang Pharmaceutical University; Gong, Ping; Zhao, Yanfang; Liu, Yajing; Zhai, Xin; US2015/307453; (2015); A1;,
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Related Products of 7781-10-4, 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. 7781-10-4, name is 4-Chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

To 1.9 g (9.2 mmol) of methyl 1H-pyrrolo[2,3-b]pyridine-3-carboxylate in 50 cm3 ofdimethylsulfoxyde under argon atmosphere, were added 1.85 g (11.0 mmol) of 4-chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidine , followed by 3.2 g (23.0 mmol) ofpotassium carbonate. The reaction mixture was heated at about 120C for 24 hours,upon which it was cooled to about 20C and treated with 200 cm3 of distilled water.The mixture was then treated with 300 cm3 and 150 cm3 of ethyl acetate and filteredon Celite. The aqueous phase was extracted with 150 cm3 of ethyl acetate. Thecombined organic extracts were dried on magnesium sulfate and concentrated todryness in vacuo (2.7 kPa). The residue was purified via column chromatography onsilica gel (0,04-0,06 mm), with dichloromethane/methanol 99:1 v/v as eluting solvent.Thus, 1.25 g of methyl 1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrrolo[2,3-b]pyridine-3-carboxylate were obtained as a light-yellow crystalline powder, mp: 207C

The synthetic route of 4-Chloro-7-methyl-7H-pyrrolo[2,3-d]pyrimidine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; AVENTIS PHARMA DEUTSCHLAND GMBH; WO2004/111048; (2004); A1;,
Chloride – Wikipedia,
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Related Products of 1871-57-4, 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. 1871-57-4, name is 3-Chloro-2-chloromethyl-1-propene belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a cooled solution (5 C) of the corresponding 4,6-O-(R)-benzylidene-d-hexopyranoside derivative (obtained using the procedure describe by our group2c) (35.4 mmol) in dry THF (70 mL) were added, successively, freshly powdered potassium hydroxide (7.0 g, 125 mmol), 18-crown-6 (0.38 g, 1.4 mmol), and 3-chloro-2-chloromethylpropene (4.1 mL, 35.4 mmol). The reaction mixture was stirred at this temperature for 3 h, and left at room temperature until all the starting material had been consumed, as monitored by TLC (5-7 days, approximately), then diluted with dichloromethane (60 mL) and washed successively with water and aqueous saturated solution of sodium bicarbonate, dried (MgSO4), filtered, and the filtrate was evaporated to dryness.

The synthetic route of 3-Chloro-2-chloromethyl-1-propene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Vega-Perez, Jose M.; Vega-Holm, Margarita; Perinan, Ignacio; Palo-Nieto, Carlos; Iglesias-Guerra, Fernando; Tetrahedron; vol. 67; 2; (2011); p. 364 – 372;,
Chloride – Wikipedia,
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These common heterocyclic compound, 4584-46-7, name is 2-Chloro-N,N-dimethylethanamine hydrochloride, 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. Recommanded Product: 2-Chloro-N,N-dimethylethanamine hydrochloride

NaN3(13.7 g, 210 mmol) was added into a solution of 2-chloro-N,N- dimethylethylamine hydrochloride (10.0 g, 70 mmol) in 100 mL water and the reaction mixture was heated to 70 C for overnight. The solution was basified with 4 M NaOH solution and extracted with anhydrous diethyl ether three times. The resulting solution was dried over MgS04 and concentrated to give volatile colorless oil. (5.9 g, 74%)1H NMR (CDC13, 400 MHz): delta 3.31 (t, 2H), 2.45 (t, 2H), 2.21 (s, 6H, N(CH3)2).

The synthetic route of 2-Chloro-N,N-dimethylethanamine hydrochloride has been constantly updated, and we look forward to future research findings.

Reference:
Patent; CORNELL UNIVERSITY; MA, Minglin; LIU, Qingsheng; (140 pag.)WO2018/140834; (2018); A1;,
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Adding a certain compound to certain chemical reactions, such as: 2613-32-3, name is 2-Chloro-4,5-difluoroaniline, 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 2613-32-3, Product Details of 2613-32-3

1-Chloro-4,5-difluoro-2-isothiocyanatobenzene To a mixture of 2-chloro-4,5-difluoroaniline (1 equiv.) and sodium hydroxide (3 equiv.) in DCM (0.24 M) and water (0.24 M) was added dropwise thiophosgene (3 equiv.) at 0 C. The reaction mixture was stirred at 25 C. overnight. TLC showed the reaction was complete. The organic phase was separated and dried over MgSO4, then concentrated to give 1-chloro-4,5-difluoro-2-isothiocyanatobenzene (53%) as a white 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, 2-Chloro-4,5-difluoroaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Signal Pharmaceuticals, LLC; Alexander, Matthew; Bahmanyar, Sogole; Hansen, Joshua; Huang, Dehua; Hubbard, Robert; Jeffy, Brandon; Leisten, Jim; Moghaddam, Mehran; Raheja, Raj K.; Raymon, Heather; Schwarz, Kimberly; Sloss, Marianne; Torres, Eduardo; Tran, Tam Minh; Xu, Shuichan; Zhao, JingJing; Boylan, John Frederick; (317 pag.)US2016/96841; (2016); A1;,
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Adding a certain compound to certain chemical reactions, such as: 623-12-1, name is 1-Chloro-4-methoxybenzene, 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 623-12-1, Safety of 1-Chloro-4-methoxybenzene

General procedure: Under an N2atmosphere, KOtBu (1.3 mmol), complex 1 (1 mol%),dioxane (2 ml), amines (1.3 mmol) and aryl chlorides (1.0 mmol)were successively added into a Schlenk tube. The mixture wasstirred vigorously at 90C for 4 h. Then the solvent was removedunder reduced pressure and the residue was purified by columnchromatography on silica gel (eluent:PE/EA = 15:1) to give the pureproducts. The reported yields are the average of two runs.The catalytic reactions have been given in Tables 4-7. The result-ing amines were identified by comparison of the1H and13C NMRdata with those previously reported (ESI).

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; Nirmala, Muthukumaran; Prakash, Govindan; Ramachandran, Rangasamy; Viswanathamurthi, Periasamy; Malecki, Jan Grzegorz; Linert, Wolfgang; Journal of Molecular Catalysis A: Chemical; vol. 397; (2015); p. 56 – 67;,
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These common heterocyclic compound, 108-41-8, name is 1-Chloro-3-methylbenzene, 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. HPLC of Formula: C7H7Cl

A mixture of 1-chloro-3-methyl benzene (126 mg, 1 mmol), thiophenol (110 mg, 1 mmol), NaOH (60 mg, 1.5 mmol) and 5 mol % NiL2 (38 mg) in DMF was stirred at 70 C for 3 h. The reaction mixture was filtered and the solvent evaporated in vacuo to give the crude product, which was purified by column chromatography (hexane/ethyl acetate=10/1) to give the title compound 3j (152 mg, 76%) as a colourless oil; [Found: C, 77.90; H, 6.12. C13H12S requires C, 77.95; H, 6.04%]; Rf=0.4 (hexane/ethyl acetate=10/1). 1H NMR (400 MHz, CDCl3): delta 7.33-7.21 (m, 9H), 2.33 (s, 3H). 13C NMR (100 MHz, CDCl3): delta 139.6, 136.2, 135.4, 131.7, 130.4, 129.4, 129.1, 128.4, 128.2, 126.7, 21.4.

The synthetic route of 1-Chloro-3-methylbenzene has been constantly updated, and we look forward to future research findings.

Reference:
Article; Gogoi, Prasanta; Hazarika, Sukanya; Sarma, Manas J.; Sarma, Kuladip; Barman, Pranjit; Tetrahedron; vol. 70; 41; (2014); p. 7484 – 7489;,
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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. 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane, A new synthetic method of this compound is introduced below., name: 1,2-Bis(2-chloroethoxy)ethane

Under nitrogen, to the mixture of (22.02 g, 199.98 mmol) in 220 mL of n- butanol, was added 46 mL of aqueous solution of LiOH H2O (18.46 g, 439.94 mmol). The mixture was heated to 95 C, followed by addition of l-chloro-2-[2-(2-chloro-ethoxy)-ethoxy] -ethane (37.43 g, 200.09 mmol) in 240 mL of n-butanol. The reaction was heated overnight, then filtrated. 1 M of aqueous hydrochloric acid was added to adjust pH to 8. After removal of most n-butanol under reduced pressure, the residue was extracted with dichloromethane 250 mL x 2. The combined organic layer was washed with brine and dried over anhydrous MgSCH. The crude product was purified by column chromatography on silica gel, giving 6.5 g of 6,7,9,10,12,13-Hexahydro- 5,8,11,14-tetraoxa-benzocyclododecene as yellow oil, 14.4% yield.

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; ZHIHONG, Chen; (142 pag.)WO2019/46163; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 20850-43-5, A common heterocyclic compound, 20850-43-5, name is 5-(Chloromethyl)benzo[d][1,3]dioxole, molecular formula is C8H7ClO2, 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 7:Preparation of compound Ig: 2-(Benzo[l,3]dioxol-5-ylmethyl-methyl-amino)-ethanol.2-(Methylamino)ethanol (22.0 g, 290 mmol) was added to a stirred solution of 3,4- methylenedioxybenzyl chloride (25.0 g, 147 mmol) in DCM (45 mL) at -780C under nitrogen. The solution was stirred for 15 minutes at -780C then warmed to room temperature and stirred for 16h. 1.2 M NaOH (100 mL) was added and the phases were separated. The organic layer was washed water (2 x 150 mL) and concentrated under vacuum to give 25.3 g (83%) of 2-(benzo[l,3]dioxol-5-ylmethyl- methyl-amino)-ethanol as a clear oil.

The synthetic route of 20850-43-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KALYPSYS, INC.; WO2007/62417; (2007); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics