Month: December 2020

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. 68327-04-8, name is (1S,2S)-2-Aminocyclopentanol hydrochloride, the common compound, a new synthetic route is introduced below. HPLC of Formula: C5H12ClNO

4-Bromo-2,6-difluoro-bezonitrile (2.5 g, 1 eq), ((1S,2S)-2-aminocyclopentanol hydrochloride (1.74 g, 1.1 eq), and DIPEA (3.3 mL, 1.1 eq) are dissolved in DMSO (30 mL), and stirred at 120 C. for 2 h. The reaction mixture is poured to saturated aqueous NH4Cl (150 mL), extracted with EtOAc (3¡Á100 mL), dried over Na2SO4, filtered, and concentrated to give 4-bromo-2-fluoro-6-((1S,2S)-2-hydroxycyclopentylamino)benzonitrile (3.4 g, 100% yield). LCMS: m/z=299, 301 [M+H]+.

The synthetic route of 68327-04-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Huang, Kenneth He; Ommen, Andy J.; Barta, Thomas E.; Hughes, Philip F.; Veal, James; Ma, Wei; Smith, Emilie D.; Woodward, Angela R.; McCall, W. Stephen; US2008/269193; (2008); A1;,
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Adding a certain compound to certain chemical reactions, such as: 2568-33-4, 3-Methylbutane-1,3-diol, 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, 2568-33-4, blongs to alcohols-buliding-blocks compound. Computed Properties of C5H12O2

Example 123(3R*,4R*)-N-[3,5-bis(trifluoromethyl)benzyl]-3-(4-fluoro-2-methylphenyl)-1-(3-hydroxy-3-methylbutyl)-N-methylpiperidine-4-carboxamide monohydrochloride(step 1)To a solution of 3-methyl-1,3-butanediol (1.0 g) in pyridine (10 mL) was added p-toluenesulfonyl chloride (2.26 g) at 0 C., and the mixture was stirred at room temperature for 27 hr. The reaction mixture was poured into ethyl acetate, organic layer was washed with 1N hydrochloric acid and water and dried, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (solvent gradient; 0?100% ethyl acetate/hexane) to give 3-hydroxy-3-methylbutyl 4-methylbenzenesulfonate (878 mg, 35%) as a colorless oil.1H-NMR (300 MHz, CDCl3):delta 1.22 (6H, s), 1.34 (1H, s), 1.86 (2H, t, J=6.8 Hz), 2.45 (3H, s), 4.21 (2H, t, J=6.8 Hz), 7.35 (2H, d, J=8.0 Hz), 7.80 (2H, d, J=8.3 Hz)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2568-33-4, its application will become more common.

Reference:
Patent; Shirai, Junya; Morimoto, Shinji; Sugiyama, Hideyuki; Sakauchi, Nobuki; Yoshikawa, Takeshi; US2008/275085; (2008); A1;,
Alcohol – Wikipedia,
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Electric Literature of 6642-34-8, The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 6642-34-8, name is (6-Bromobenzo[d][1,3]dioxol-5-yl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: In an oven dried Schlenk tube, were added alcohol 1 (100.0mg, 0.31-0.53mmol), ethyl acrylate [155.1-265.3mg, (i.e., 1.55-2.65 mmol)], and Cs2CO3 [303.0-518.0mg, (i.e., 0.93-1.59mmol)] followed by the addition of toluene (2mL) at rt under nitrogen atmosphere. The resulted reaction mixture was stirred at 50C in an oil bath for 48h. After the completion of Michael addition (monitored by TLC) and to the cooled reaction mixture at rt, were added Pd(OAc)2 (6.9-11.9mg, 10mol%) and PPh3 (16.3-27.8mg, 20mol%) under nitrogen atmosphere. The reaction mixture was then heated at 80C in an oil bath for 24h. Once after formation intermolecular Heck coupling product, (monitored by TLC) and then to the cooled reaction mixture at rt, was added DMF (3mL) and heated to 120C, in an oil bath for 12h (monitored by TLC). The reaction mixture at rt was quenched by the addition of aqueous NH4Cl and extracted with DCM (3¡Á15mL). The organic layers were washed with saturated NaCl solution, dried (Na2SO4), and filtered. Evaporation of the solvent under reduced pressure and purification of the crude material by silica gel column chromatography (petroleum ether/ethyl acetate) furnished the lactenones 5 (40-48%).

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 6642-34-8, (6-Bromobenzo[d][1,3]dioxol-5-yl)methanol.

Reference:
Article; Reddy, A. Gopi Krishna; Krishna; Satyanarayana; Tetrahedron; vol. 69; 47; (2013); p. 10098 – 10107;,
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Adding a certain compound to certain chemical reactions, such as: 111-90-0, Diethylene Glycol Monoethyl Ether, 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, 111-90-0, blongs to alcohols-buliding-blocks compound. Recommanded Product: Diethylene Glycol Monoethyl Ether

Example 89b; Sodium hydride (60% in oil, 40 mg) was added to a mixture of 2-chloro-4-oxo-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,4-dihydro-5H-pyrrolo[3,2-d]pyrimidine-5-carbaldehyde (150 mg) obtained in Example 89a), 2-(2-ethoxyethoxy)ethanol (134 mg) and N,N-dimethylformamide (3 ml), and the resulting mixture was stirred for one hour at room temperature. Furthermore, 2-(2-ethoxyethoxy)ethanol (134 mg) and sodium hydride (60% in oil, 40 mg) were sequentially added thereto, and the resulting mixture was stirred for 15 hours at 100 C. The reaction mixture was returned to room temperature, and then the solvent was distilled off under reduced pressure. The residue was diluted with ethyl acetate, and the dilution was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was purified by chromatography, and was recrystallized from a mixed solvent of ethyl acetate/hexane. Thus, the title compound (85 mg) was obtained as a white powder.1H NMR (300 MHz, CHLOROFORM-d) delta ppm 1.18 (3H, t, J=8.2 Hz), 3.36-3.52 (6H, m), 3.68 (2H, dd, J=5.7, 3.8 Hz), 4.40 (2H, q, J=8.2 Hz), 4.45-4.52 (2H, m), 6.33-6.41 (1H, m), 7.04(2H, d, J=9.1 Hz), 7.17-7.25 (3H, m), 9.51 (1H, br. s.).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,111-90-0, its application will become more common.

Reference:
Patent; Suzuki, Hideo; Fujimoto, Takuya; Yamamoto, Takeshi; US2010/190747; (2010); A1;,
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Related Products of 2566-44-1, 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.2566-44-1, name is 2-Cyclopropylethanol, molecular formula is C5H10O, molecular weight is 86.13, as common compound, the synthetic route is as follows.

a) 500 mg (2.01 mmol) 6-Hydroxy-3,4-dihydro-1 H-isoquinoline-2-carboxylicacid tertbutyl ester, 173 mg (2.01 mmol) 2-cyclopropylethanol and 526 mg (2.01 mmol) triphenylphosphine in 5 mL THF are stirred at 000 under inert gas atmosphere. Then420 iL (2.01 mmol) diisopropylazodicarboxylate are added slowly and the reaction mixture is stirred at r.t. over night. After that time, the reaction mixture is filtered, concentrated and the residue purified by H PLC. 019 H27 N 03ES I-MSR (H PLC):(M = 317.4g/mol) 318 [M+H]1.12 mm (method A)

Statistics shows that 2566-44-1 is playing an increasingly important role. we look forward to future research findings about 2-Cyclopropylethanol.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; ROTH, Gerald Juergen; FLECK, Martin; HAEBEL, Peter Wilhelm; HEIMANN, Annekatrin; HEINE, Niklas; (172 pag.)WO2016/41845; (2016); A1;,
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Application of 617-94-7, 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. 617-94-7, name is 2-Phenyl-2-propanol. A new synthetic method of this compound is introduced below.

To sodium hydride (60% dispersion in mineral oil, 280 mg, 7.00 mmol, 0.5 equiv) in anhydrous diethyl ether (28 mL) was added freshly distilled 2-phenyl-2-propanol (4.20 g, 30.8 mmol, 2.2 equiv) at 0 C and the mixture was stirred for 1 h at room temperature. The reaction mixture was cooled to 0 C, 2,2,2-trichloroacetonitrile (2.80 mL, 28.0 mmol, 2.0 equiv) were added slowly and stirring was continued for 3 h at ambient temperature. The solvent was removed under reduced pressure and the residue re-dissolved in PE (7.0 mL), anhydrous MeOH (283 pL, 7.00 mmol, 0.5 equiv) was added and the solution was stirred for 10 min at room temperature. The mixture was filtered through a plug of Celite eluting with PE and the filtrate was concentrated in vacuo to give the crude imidate. To a suspension of Fmoc-Ala-OH (4.36 g, 14.0 mmol, 1.0 equiv) in CH CI (80 mL) was added a solution of the imidate in CH CI (15 mL) and the mixture was stirred for 16 h at room temperature. The reaction mixture was filtered through a plug of Celite eluting with CH CI , the solvent was removed in vacuo, and the residue was purified by column chromatograph (S O , PE/EtOAc 4:1) to give Fmoc-Ala-OCumyl (55) (6.00 g, 14.0 mmol, quant yield) contaminated with small amounts of 2-phenyl-2-propanol (~85:15 by 1H N MR) as a pale-yellow oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,617-94-7, 2-Phenyl-2-propanol, and friends who are interested can also refer to it.

Reference:
Patent; UNIVERSITY OF WARWICK; SHIPMAN, Michael; (96 pag.)WO2019/186174; (2019); A1;,
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Reference of 115-20-8, 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 115-20-8 as follows.

Preparation of 12′- (2, 2,2-Trichloroethylcarbonyl) vinblastine Trifluoroacetate [00125] Carbon monoxide was bubbled through a solution of 12′- iodovinblastine (53 mg, 0.057 mmol), triethylamine (57 mg, 0.565 mmol) and bis (triphenylphosphine) palladium (II) dichloride (8 mg, 0.011 mmol) in a mixture of DMF/2,2, 2-trichloroethanol (2 mL, 1 : 1) for 5 min, then the reaction mixture was heated at 50 C for 9 h under one atmosphere of carbon monoxide (balloon). The solution was diluted with ethyl acetate (15 mL) then washed with saturated aqueous NaHC03 (2 x 5 mL) and brine (5 mL), dried over MgS04 and evaporated to dryness in vacuo. The residue was purified by reverse phase chromatography (C18, acetonitrile/water, 0.05% trifluoroacetic acid) to provide 12′- (2, 2,2- trichloroethylcarbonyl) vinblastine trifluoroacetate (33 mg, 48%) as a white powder after lyophilization

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,115-20-8, its application will become more common.

Reference:
Patent; AMR TECHNOLOGY, INC.; WO2005/55939; (2005); A2;,
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Reference of 629-30-1, 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.629-30-1, name is 1,7-Heptanediol, molecular formula is C7H16O2, molecular weight is 132.2, as common compound, the synthetic route is as follows.

7- bromoheptane-l-ol1 (2): Heptane- 1,7-diol (36.0 g, 272 mmol; Alfa Aesar) and aq. 48% HBr (38 mL, 0.9 equiv.) were heated under reflux in benzene (400 mL) with water removal using a Dean-Stark apparatus. After 16 h, all volatiles were removed in vacuo and the residue was purified by Si02 column chromatography using a gradient of 10-30% EtOAc/hexanes as eluent to give 7-bromoheptan-l-ol (26.22 g, 62%) as a colorless oil. TLC: 50% EtOAc/hexanes, Rf ~ 0.40; NMR (400 MHz, CDC13) delta 3.61 (t, 2H, J = 7.1 Hz), 3.39 (t, 2H, J= 6.8 Hz), 1.80- 1.88 (m, 2H), 1.52-1.58 (m, 2H), 1.30-1.46 (m, 6H).

The chemical industry reduces the impact on the environment during synthesis 629-30-1, I believe this compound will play a more active role in future production and life.

Reference:
Patent; MCW RESEARCH FOUNDATION, INC.; IMIG, John, David; CAMPBELL, William, B.; FALCK, John, Russell; WO2012/138706; (2012); A1;,
Alcohol – Wikipedia,
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Electric Literature of 2516-33-8 , The common heterocyclic compound, 2516-33-8, name is Cyclopropylmethanol, molecular formula is C4H8O, 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.

b) 5-Bromo-6-cyclopropylmethoxy-pyridine-2-carboxylic acid Sodium hydride (4.83 g, 0.12 mol) was added into cyclopropanemethanol (CAN 2516-33- 8, 30 g) at 0 C and the mixture was stirred at 0 C for 1 h. Then to the mixture was added5 methyl 5-bromo-6-chloro-pyridine-2-carboxylic acid methyl ester (3 g, 12.75 mmol). The obtained solution was heated to 90 C for 2 h. Then the mixture was evaporated to dryness, the residue was dissolved in 40 mL of water, and adjusted to pH = 4 with hydrochloric acid (3 N), and extracted with ethyl acetate (3 x 30 mL). The combined organic layer was washed with water (2 x 30 mL) and brine (2 x 50 mL) then evaporated to dryness to obtain10 the product as a white solid (2.5 g, 76.7%); MS (El): mle = 272.0 [MH?i.

The synthetic route of 2516-33-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; FREI, Beat; GOBBI, Luca; GRETHER, Uwe; KIMBARA, Atsushi; NETTEKOVEN, Matthias; ROEVER, Stephan; ROGERS-EVANS, Mark; SCHULZ-GASCH, Tanja; WO2014/86705; (2014); A1;,
Alcohol – Wikipedia,
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Adding a certain compound to certain chemical reactions, such as: 23783-42-8, 2,5,8,11-Tetraoxatridecan-13-ol, 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: 2,5,8,11-Tetraoxatridecan-13-ol, blongs to alcohols-buliding-blocks compound. Recommanded Product: 2,5,8,11-Tetraoxatridecan-13-ol

A method of synthesizing the silybin phenolic ether derivatives as shown in Formula I-d is as follows:1) Add 8.00 g (0.20 mol) NaOH, 80 ml water to a 250 ml three-necked flask.Stir to dissolve it evenly. 24.96 g (0.12 mol) of tetraethylene glycol monomethyl ether was added to 50 ml of THF to be uniformly dissolved, then added to the above-mentioned three-necked flask and uniformly mixed with the NaOH solution.The mixture was stirred in an ice bath at 0 55 C. and thoroughly deoxygenated with nitrogen. 22.88 g (0.12 mol) of p-toluenesulfonyl chloride and 40 ml of THF were mixed well, and then slowly added dropwise to the above three-necked flask. The dropping process kept the temperature of the reaction liquid. After exceeding 10C, the reaction was continued for 6 hours after completion of the dropwise addition to stop the reaction.The reaction solution was extracted three times with diethyl ether, and the ether extract was washed with water until neutral and then dried over anhydrous magnesium sulfate. After filtration and rotary evaporation, the ether was removed.This gave 40.83 g (yield: 94%) of the corresponding p-toluenesulfonate of formula III-b,

The synthetic route of 23783-42-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Physics And Chemistry Technology Institute; Zhao Yuxia; He Ru; Wu Feipeng; (18 pag.)CN105037337; (2018); B;,
Alcohol – Wikipedia,
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