Tag: M.W=200-300

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. 149965-40-2, name is (5-Bromo-2-chlorophenyl)methanol, the common compound, a new synthetic route is introduced below. Formula: C7H6BrClO

(2) To a solution of 2.08 g (9.39 mol) of 5-bromo-2-chlorobenzylalcohol in 30 ml of dry diethyl ether was added dropwise 1.27 g (4.23 mmol) of phosphorous tribromide with ice-cooling. The mixture was stirred with ice-cooling for 3 hours and stirred at room temperature for 1.5 hours. To the reaction solution were added ice water and then tert-butyl methyl ether. The mixture was stirred for 30 minutes and separated. The organic layer was washed successively with an about 5% aqueous solution of sodium bicarbonate and water, then dried and concentrated. The solid residue (1.99 g) was subjected to silica gel column chromatography (eluted with n-hexane) to obtain 1.88 g of 5-bromo-2-chlorobenzylbromide as flocculent crystals.

The synthetic route of 149965-40-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Company, Limited; US6489487; (2002); B1;,
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Electric Literature of 1454-85-9, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.1454-85-9, name is Heptadecan-1-ol, molecular formula is C17H36O, molecular weight is 256.4672, as common compound, the synthetic route is as follows.

General procedure: The D1-OCn (n =15-21) were prepared as reported previously.22,23 The alkyl alcohol (1mmol) with triethylamine (2mmol) was added to isobutenyl binaphthyl di(acid chloride) (0.5mmol) in THF, and stirred at 60 °C for 1 day. After the evaporation of the solvent, the product was purified by silica gel column chromatography with CHCl3 as an eluent.

The chemical industry reduces the impact on the environment during synthesis 1454-85-9, I believe this compound will play a more active role in future production and life.

Reference:
Article; Kikkawa, Yoshihiro; Ishitsuka, Manami; Omori, Kazuhiro; Kashiwada, Ayumi; Tsuzuki, Seiji; Hiratani, Kazuhisa; Bulletin of the Chemical Society of Japan; vol. 88; 6; (2015); p. 834 – 842;,
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Adding a certain compound to certain chemical reactions, such as: 575-03-1, 7-Hydroxy-4-(trifluoromethyl)coumarin, 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, Product Details of 575-03-1, blongs to alcohols-buliding-blocks compound. Product Details of 575-03-1

General procedure: To a magnetically-stirred solution of 7-hydroxycoumarin derivatives (2 mmol), aromatic aldehydes (2 mmol) and NEt3 (2 mmol) in THF (8 mL) a mixture of dialkyl acetylenedicarboxylate (2 mmol) in THF (2 mL) was added in 15 min. The reaction mixture was then allowed to stand at room temperature for 0.5-10 h. After completion of the reaction as indicated by thin-layer chromatography (TLC) (n-hexane/EtOAc, 1:1), the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (Merck, 230-400 mesh) using a mixture of n-hexane/EtOAc (1:1) as eluent to afford the pure product as a light yellow powder.

The synthetic route of 575-03-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Asghari, Sakineh; Baharfar, Robabeh; Darabi, Samaneh Ahangar; Mohammadian, Reza; Journal of the Brazilian Chemical Society; vol. 26; 2; (2015); p. 218 – 223;,
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Electric Literature of 2215-78-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 2215-78-3, name is (4-Phenoxyphenyl)methanol, molecular formula is C13H12O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

4-Phenoxybenzyl alcohol (20.0 g) was dissolved in toluene (100 mL), and thionyl chloride (13.1 g) was added to the solution over 30 minutes at room temperature. After 2 hours, the reaction solution was concentrated under reduced pressure. The residue was distilled to give 16.7 g (yield: 76%) of the target product. A boiling point thereof was 137 C/3 mmHg.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 2215-78-3, (4-Phenoxyphenyl)methanol.

Reference:
Patent; Agro Kanesho Co Ltd; Aizawa, Ryo; Okada, Itaru; (13 pag.)KR2016/85330; (2016); A;,
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Electric Literature of 31952-16-6, Adding some certain compound to certain chemical reactions, such as: 31952-16-6, name is 2,2-Dibenzylpropane-1,3-diol,molecular formula is C17H20O2, 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 31952-16-6.

To a solution of (PhCH2)2C(CH2OH)2 (14.4 g, 0.06 mol) in 40 mL of anhydrous pyridine at 0 C was added with stirring under an inert atmosphere 16 mL (26 g, 0.21 mol) of SOCl2 in ca. 2 h. The resulting mixture was refluxed for 2 h and then stirred at room temperature for 15 h. After cooling to 0 C, equal volumes of CH2Cl2 and water (200 mL each) were added to the reaction mixture. The separated organic layer was washed with an aqueous solution of HCl (pH 4) and then with distilled water. After the CH2Cl2 solution was treated with sodium sulfate, the solvent was removed under reduced pressure. To the resulting oily residue was added ethyl ether (30 mL) until an off-white solid precipitated, which was recrystallized from ethanol to give 10 g of crystalline (PhCH2)2C(CH2Cl)2 (61% yield). 1H NMR (CDCl3, 20 C, 200.13 MHz): d 7.5-7.2 (m, 10 H, Ph), 3.23 (s, 4 H,CH2Cl), 2.91 (s, 4 H, CH2Ph).

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. 31952-16-6, 2,2-Dibenzylpropane-1,3-diol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; CONSIGLIO NAZIONALE DELLE RICERCHE; EP941230; (2004); B1;,
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As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 517-21-5, name is Sodium 1,2-dihydroxyethane-1,2-disulfonate, molecular formula is C2H4Na2O8S2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. name: Sodium 1,2-dihydroxyethane-1,2-disulfonate

Glyoxal-sodium bisulfite (2.72 g, 10.2 mmol) was added to a solution of 3-amino-5-methyl-1H-pyrazole (2 g, 20.6 mmol) in water (40 mL) and was heated to 70 C. for 25 min. The mixture was then cooled down to room temperature and sodium cyanoborohydride (2.73 g, 43.4 mmol) was added and the mixture was stirred overnight. Methanol (70 mL) was added and the mixture was stirred for 1 h. Concentrated hydrochloric acid (12 N) was added until a pH<2 was obtained and the resulting mixture was stirred at room temperature overnight. The solution was then neutralized with an aqueous solution of sodium hydroxide (1M) and the solvent was evaporated. The residue was resuspended in methanol (40 mL) and stirred for 1 h. After filtration, the solvent was evaporated and the residue was purified by chromatography on a silica gel column (eluent: EtOAc, EtOAc-MeOH, 95:5, 90:10); N1,N2-bis(5-Methyl-1H-pyrazol-3-yl)ethane-1,2-diamine was obtained as a white solid.1H NMR (400 MHz, CDCl3): delta=2.21 (s, 6H), 3.35 (s, 4H), 5.35 (s, 2H).13C NMR (100 MHz, CDCl3/CD3OD 10:1): delta=11.29, 43.86, 89.75, 142.32, 155.13.MS (ESI): m/z=221 (MH+). With the rapid development of chemical substances, we look forward to future research findings about 517-21-5. Reference:
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Synthetic Route of 4654-39-1, Adding some certain compound to certain chemical reactions, such as: 4654-39-1, name is 2-(4-Bromophenyl)ethanol,molecular formula is C8H9BrO, 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 4654-39-1.

A solution of 2-(4-bromophenyl)ethanol (4.43 g, 0.0220 mol) dissolved in CH2Cl2 (50 mL) was cooled to 0C. Next, PPh3 (6.92 g, 0.0264 mol) was added, followed by NBS (4.70 g, 0.0264 mol), and vigorous effervescence in a yellow solution was observed. The mixture was allowed to stir at 0C for 60 minutes. After this time, the yellow solution was treated with saturated sodium bicarbonate solution (20 mL). The deep, dark blue organic layer was separated, and the aqueous layer was extracted with CH2Cl2 (2 × 20 mL). The organic layers were combined and then the solvent was removed under reduced pressure to yield a deep, dark blue oil. The oil was purified on a column of silica (~1.5 cm × 20 cm) using EtOAc/hexanes (1:10) as an eluent and collecting the first nearly colourless fraction. Removal of the volatiles under reduced pressure yielded a very pale orange liquid. Yield: 5.38 g (93%). 1H NMR (500 MHz, 22C, CDCl3): 7.43 (d, 2H, 2JHH = 8 Hz, Ar), 7.08 (d, 2H, 2JHH = 8 Hz, Ar), 3.53 (t, 2H, 3JHH = 7 Hz, -CH2CH2-), 3.11 (t, 2H, 3JHH = 7 Hz, -CH2CH2-).

According to the analysis of related databases, 4654-39-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Tassone, Joseph P.; Mawhinney, Robert C.; Spivak, Gregory J.; Journal of Organometallic Chemistry; vol. 776; (2015); p. 153 – 156;,
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Reference of 124937-73-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 124937-73-1, name is 3-(2-Methoxy-5-methylphenyl)-3-phenylpropan-1-ol, molecular formula is C17H20O2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Example 1: Preparation of 3-(2-methoxy-5-methylphenyl)-3-phenylpropyl methane sulfonate (Vb)This intermediate is of significant importance for use in the preparation of Tolterodine or salts thereof, or its derivatives according to the present invention.In a 3-necked round bottom flask, 6-methyl-4-phenyl-3,4-dihydro coumarin (II, 10Og, 0.420 mol) is charged into methanol (500 ml) at about 250C with stirring. To the resulting suspension, potassium carbonate (K2CO3, 87 g, 0.63 mol) and methyl iodide (MeI, 78 ml, 1.25 mol) are added and the mass is stirred at from about 550C to about 6O0C for 4 h. The reaction mass is cooled to from about 400C to about 450C and MeI (27 ml, 0.43 mol) and K2CO3 (29 g, 0.21 mol) are added. Re-heat the mass to 55~ 6O0C and stir for additional 6 h until the reaction completes. Then solvent is removed by distillation under vacuum. The residue is dissolved in 350 ml of toluene. This organic phase is washed once with 750 ml of DM water and twice with 450 ml of DM water.The organic layer thus obtained is charged into a 3-necked round bottom flask under N2 atmosphere and cooled at temperature from about -50C to about 5C. Toluene solution of sodium bis(2-methoxyethoxy) aluminum hydride (Red-Al, 200 ml, 70% w/v, 0.706 mol) is slowly added through a dropping funnel over a period of 120 min, maintaining the solution temperature within -5 ~ 50C. The mixture is stirred for an additional 1 h at this temperature until the reaction completes. Then aqueous solution of NaOH (80 ml, 10%) is added through a dropping funnel over a period of 45 min, maintaining the temperature at 0 ~ 100C, and continue stirring for an additional 45 min at the same temperature. Add 750 ml of DM water and stir for 30 min at 250C. The biphasic reaction mass is filtered through a celite bed (10 g). The organic layer is collected and dried over 20 g of anhydrous sodium sulfate (Na2SO4). The solids are filtered and washed with 50 ml of toluene. The toluene is distilled off completely and compound IV is obtained as slightly yellow thick oil.The thick oil is dissolved in 300 ml of dichloromethane (DCM) under N2 atmosphere. Triethylamine (Et3N, 90 ml, 0.647 mol) is added and the mass is cooled to 0 ~ 5C. Mesyl chloride (MsCl, 36 ml, 0.465 mol) is added slowly through a dropping funnel over a period of 120 min, keeping the solution temperature below 1O0C. Continue stirring the mixture for an additional 1 h at 0~5C until the reaction completes. 1 L of cold DM water (0~5C) was added and the mass is stirred for 30 ~ 60 min at this temperature. Cone. HCl (25 ml) is added and the mass is stirred until it reaches 25C. The organic layer is collected and washed with 200 ml of DM water. About 180 ~ 220 ml of DCM is distilled off from the organic layer under atmosphere pressure at 38 ~ 43C. 400 ml of cyclohexane is added to the residue and the mass is heated to reflux till a clear solution is obtained (70 ~ 800C). This solution is cooled slowly and compound Vb crystallized. The solid is filtered in Buchner funnel and spray washed with 100 ml of cold cyclohexane. The mass is dried under vacuum at 600C to give 90 ~ 110 g of title compound.

According to the analysis of related databases, 124937-73-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; PHARMATHEN S.A.; KOFTIS, Theoharis, V.; NEOKOSMIDIS, Efstratios; SONI, Rohit, Ravikant; MANDALOU, Panagiota; MENISIOU, Aristotelis; WO2010/94292; (2010); A1;,
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Adding a certain compound to certain chemical reactions, such as: 7735-42-4, 1,16-Hexadecanediol, 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, Recommanded Product: 7735-42-4, blongs to alcohols-buliding-blocks compound. Recommanded Product: 7735-42-4

Synthesis Example C-(18) 1,16-Hexadecanediol (13.75 g) was dissolved in 37 ml of cyclohexane, and 57% hydrobromic acid solution (37 ml) was added to this solution. The reaction mixture was refluxed for six hours while stirring. After the reaction, the mixture was extracted three times with diethyl ether. The organic layer was neutralized with saturated sodium hydrogen carbonate solution, washed with saline solution, dried over magnesium sulfate, and filtered, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel flash chromatography (hexane: ethyl acetate = 7:3) gave 16-bromohexadecan-1-ol as white crystals at a 67% yield. Molecular weight: 320.9 (C16H33BrO) TLC: (hexane-ethyl acetate 7-3) Rf value=0.53 1H-NMR: (300MHz, CDCl3)delta: 1.26 (s large, 24H, -(CH2)12-); 1.56 (qt, 2H, J=7.2Hz, -CH2-); 1.85 (qt, 2H, J=7.1 Hz, -CH2-); 3.40 (t, 2H, J=7.1Hz, -CH2-Br); 3.63 (t, 2H, J=6.6Hz, -CH2-O-) 13C-NMR: (75MHz, CDCl3) delta: 25.84; 27.28; 28.22; 29.48-29.50; 32.90; 33.20; 34.01; 63.01

At the same time, in my other blogs, there are other synthetic methods of this type of compound,7735-42-4, 1,16-Hexadecanediol, and friends who are interested can also refer to it.

Reference:
Patent; Meiji Dairies Corporation; EP1854777; (2007); A1;,
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Related Products of 162358-05-6, 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. 162358-05-6, name is 2-(4-Octylphenyl)ethanol. A new synthetic method of this compound is introduced below.

Example 6 Preparation of Compound of Formula VIIIn a round bottom flask, 600 ml of methylene chloride was charged and 100 gm of compound of Formula V, obtained as in Example 4, and 5.0 gm of DMAP and 110 gm of triethyl amine was added. The reaction mass was stirred for about 10 minutes and cooled at about 0-5 C. 75 gm of methane sulphonyl chloride was added at about 0-5 C. and the temperature of reaction mass was raised to about 25-30 C. The reaction mass was stirred at about 25-30 C. for about 1 hour and water (500 ml) was added to the reaction mass. The pH was adjusted to about 2-4 by using aq. HCl and the reaction mass was stirred for about 20 min. The organic layer was separated and washed with 7% bicarbonate solution followed by washing with brine. The organic layer was treated with charcoal and distilled out under vacuum and degassed to get 110 gm of compound of Formula VI.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,162358-05-6, 2-(4-Octylphenyl)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; Glenmark Generics Limited; Gharpure, Milind; Narawade, Krishna; Chand, Prem; Bhirud, Shekhar; US2015/18578; (2015); A1;,
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