Month: March 2021

Related Products of 101-32-6, 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. 101-32-6, name is 2,2-(Benzylimino)diethanol. A new synthetic method of this compound is introduced below.

Synthesis was performed according to the published procedure[17] with some alterations as mentioned below. 2,2′-(Benzylazanediyl)bis(ethan-1-ol) (759 mg, 3.89 mmol) in anhydrous THF (40 mL) was transferred into the two-necked flask under argon atmosphere. A solution of 1 M potassium tert-butoxide in THF(8.03 g, 71.56 mmol) was slowly injected into the reaction mixture. Pentaethylene glycol di(p-toluenesulfonate) (2.12 g, 3.89 mmol) was dissolved in anhydrous THF (20 mL) and added to the reaction mixture dropwise. The mixture was stirred for 2.5 h at 40 C. TLCanalysis (ethyl acetate/MeOH 5:1, Rf of 4 = 0.29) indicated that thereaction was completed immediately. THF was evaporated under reduced pressure. The product was dissolved in ethyl acetate (50 mL) and extracted with 5% hydrochloric acid (v/v) (3 x 50 mL).T he water layer was collected, and neutralized by 1 M NaOH and the product was extracted three times with ethyl acetate(3 x 80 mL). The organic layer was collected and evaporated todryness. The crude product was purified by column chromatographyon silica with ethyl acetate/MeOH/TEA 15:1:0.1 as an eluent. After some impurities were washed out, the mobile phase was changed to ethyl acetate/MeOH/TEA 15:3:1 as the eluent. Yield: 792 mg (51%) of colorless oil. 1H NMR (500 MHz, CDCl3, 25 C):d 2.74-2.93 (m, 4H, CH2), 3.59-3.72 (m, 26 H, CH2) and 7.22e7.41 ppm (m, 5 H, Bn-H); MS (APCI): m/z 398.7 [MH]. The other analytical data corresponded well with data published in the literature

At the same time, in my other blogs, there are other synthetic methods of this type of compound,101-32-6, 2,2-(Benzylimino)diethanol, and friends who are interested can also refer to it.

Reference:
Article; Lochman, Lukas; Svec, Jan; Roh, Jaroslav; Novakova, Veronika; Dyes and Pigments; vol. 121; (2015); p. 178 – 187;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Synthetic Route of 39590-81-3, Adding some certain compound to certain chemical reactions, such as: 39590-81-3, name is 1,1-Bis(Hydroxymethyl)cyclopropane,molecular formula is C5H10O2, 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 39590-81-3.

Step 1; Synthesis of 1,1-bis(methanesulfonyloxymethyl)cyclopropane 1,1-Bishydroxymethylcyclopropane(3.0 g, 29.4 mmol) in 40 ml of dichloromethane was mixed with triethylamine (11.9 g, 118 mmol), and methanesulfonyl chloride (10.1 g, 88.2 mmol) was added dropwise with cooling with ice. The reaction solution was stirred for 2 hours while it was gradually warmed to room temperature. After the reaction, chloroform and water were added, and the organic layer was separated, washed with water, then dried with saturated aqueous sodium chloride and over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (n-hexane/ethyl acetate = 9/1 to 1/1) to obtain 2.85 g of the desired product 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. 39590-81-3, 1,1-Bis(Hydroxymethyl)cyclopropane, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Nissan Chemical Industries, Ltd.; EP2336104; (2011); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Electric Literature of 35106-82-2 ,Some common heterocyclic compound, 35106-82-2, molecular formula is C9H10O, 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 1: 1-(chloromethyl)-2-vinylbenzene A solution of (2-vinylphenyl)methanol (3.10 g, 23.1 mmol) in DCM (30 mL) was cooled down to 0¡ã C., and then added MsCl (2.01 mL, 27.7 mmol) dropwise. The resulted mixture was stirred at room temperature for overnight. After the mixture was diluted with DCM (50 mL), the organic layer was washed with H2O (30 mL*2), saturated NaHCO3 aqueous solution and brine successively, then dried over sodium sulfate, filtered and concentrated to afford 1-(chloromethyl)-2-vinylbenzene (2.92 g, yield: 83percent) as colorless oil, which can directly used for next step.

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. 35106-82-2, (2-Vinylphenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; SHANGHAI DE NOVO PHARMATECH CO. LTD.; GAO, Daxin; YANG, Heping; WANG, Pei; (84 pag.)US2017/37038; (2017); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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.18068-06-9, name is 4-Methoxycyclohexanol, molecular formula is C7H14O2, molecular weight is 130.19, as common compound, the synthetic route is as follows.Computed Properties of C7H14O2

To a mixture of 5 g aluminiumtrichloride (37.5 mmol) and 9.32 ml of lithiumaluminiumhydride in diethylether (1 M) is added a solution of 4.8 g 4-methoxy- cyclohexanol (36.8 mmol ,cis/trans-mixture) in 5 ml of diethylether. The reaction mixture is stirred for 20 minutes at room temperature and then concentrated in vacuo. Diethylether is added and decanted off several times. Diethylether is added to the residue and then sulfuric acid (10%) is added until both phases are clear. The organic phase is separated and extracted consecutively with water and saturated sodium bicarbonate solution. The organic phase is dried.Yield: 1 .33 g (28%)ESI mass spectrum: m/z = 131 (M+H)+

At the same time, in my other blogs, there are other synthetic methods of this type of compound,18068-06-9, 4-Methoxycyclohexanol, and friends who are interested can also refer to it.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; HECKEL, Armin; HIMMELSBACH, Frank; LEHMANN-LINTZ, Thorsten; REDEMANN, Norbert; SAUER, Achim; THOMAS, Leo; BLACK, Phillip; BLACKABY, Wesley; DANILEWICZ, John; LINNEY, Ian; AUSTEN, Matthias; SCHNEIDER, Martin; SCHREITER, Kay; WO2011/104338; (2011); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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. 1467-84-1, name is (trans-4-Aminocyclohexyl)methanol, molecular formula is C7H15NO, 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. Recommanded Product: (trans-4-Aminocyclohexyl)methanol

To a stirred solution of 2,4-dichloro-5-nitropyrimidine (0.6 g, 3 mmol) in THF (10 mL) was added DIPEA (0.4 g, 3 mmol) dropwise followed by ((1R,4R)-4-aminocyclohexyl)methanol (0.4 g, 3 mmol) at ambient temperature. The reaction mixture was stirred at ambient temperature for 4 h. Completion of the reaction was confirmed by UPLC. The product was isolated to afford ((1R, 4R)-4-((2-chloro-5-nitropyrimidin-4-yl)amino)cyclohexyl)methanol (0.3 g, 33%) as a yellow solid. MS (ESI) m/z 287 [M+1]+.

With the rapid development of chemical substances, we look forward to future research findings about 1467-84-1.

Reference:
Patent; Celgene Corporation; CANAN, Stacie S.; HAWRYLUK, Natalie Anne; WITTY, Michael John; (74 pag.)US2017/348315; (2017); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 873-76-7, (4-Chlorophenyl)methanol, 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, Safety of (4-Chlorophenyl)methanol, blongs to alcohols-buliding-blocks compound. Safety of (4-Chlorophenyl)methanol

General procedure: 0.5 mmol substrate, 1.5 mmol NH4OAc, 0.15 mmol TEMPO, 2 mL AcOH and 0.15 mmol HNO3 weresuccessively added to a dried 45 mL tube filled with 1atm oxygen. Then the reaction tube was sealed andplaced in a constant-temperature oil bath to perform the reaction for 12 h. Once the reaction time wasreached, the mixture was cooled to room temperature. Then the mixture was alkalized to pH 7-8 with sodiumhydroxide aqueous solution. GC analysis of organic phase provided the GC yields of the products.Subsequently, the crude product from another parallel experiment was purified by column chromatography,and identified by 1H-NMR, 1C-NMR or GC-MS

The synthetic route of 873-76-7 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhao, Bo; Ren, Yun-Lai; Ren, Fangping; Tian, Xinzhe; Zhao, Shuang; Letters in Organic Chemistry; vol. 15; 7; (2018); p. 627 – 632;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Related Products of 17100-58-2, 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 17100-58-2, name is (4-Bromo-2-methylphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows.

4-Bromo-1-bromomethyl-2-methyl-benzene (Intermediate 138) A solution of (4-bromo-2-methyl-phenyl)-methanol (Intermediate 133, 319.0 mg, 1.58 mmol) and triphenylphosphine (466.0 mg, 1.74 mmol) in 5 mL CH2Cl2 was cooled to 0 C. and N-bromosuccinimide (309.0 mg, 1.74 mmol) was added in 5 portions over 20 minutes. The solution was warmed to 25 C. and stirred for 17 hours. The reaction was quenched by the addition of dilute aqueous NaHCO3. The resulting mixture was extracted with Et2O and the combined organic layers were washed with H2O and saturated aqueous NaCl before being dried (Na2SO4) and concentrated under reduced pressure. The title compound, 350.0 mg (84%), was isolated by column chromatography (2-3% EtOAc-hexanes) as a colorless oil. 1H NMR (CDCl3) delta: 7.32 (1H, d, J=2.0 Hz), 7.29 (1H, dd, J=2.0, 7.9 Hz), 7.15 (1H, d, J=7.9 Hz), 4.43 (2H, s), 2.37 (3H, s).

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 17100-58-2, (4-Bromo-2-methylphenyl)methanol.

Reference:
Patent; Allergan Sales, Inc.; US6313107; (2001); B1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Synthetic Route of 110-73-6, 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. 110-73-6, name is 2-(Ethylamino)ethanol, molecular formula is C4H11NO, 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.

To a flask under a nitrogen atmosphere15 g (1 eq) of 4,4-difluorobenzophenone and 31.1 g of 2-ethylamino ethanol (5 eq) was added thereto,And the temperature was raised while stirring at 160 C.The reaction was carried out at 160 DEG C for 48 hours and then cooled to room temperature.Distilled water was added thereto, followed by extraction with methylene chloride or ethyl acetate, followed by drying under reduced pressure.The residue was recrystallized from ethyl acetate at room temperature to obtain an off-white Compound A. (20 g, 82% yield)

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 110-73-6, 2-(Ethylamino)ethanol.

Reference:
Patent; LG CHEM, LTD.; Lee, Dami; Park, Jong-Ho; (30 pag.)KR2017/3170; (2017); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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. 2854-16-2, name is 1-Amino-2-methylpropan-2-ol, the common compound, a new synthetic route is introduced below. Recommanded Product: 2854-16-2

To a solution of 2-fluorobenzene-1-sulfonyl chloride (15 g, 77 mmol) in tetrahydrofuran (THF) (300 ml.) at 0C was added potassium carbonate (13.85 g, 100 mmol), water (110 ml.) and 1-amino-2-methylpropan-2-ol (6.87 g, 77 mmol) and was stirred for 4 h at 25 C. The reaction mixture was quenched with ice cold water (200 mL) and extracted with ethyl acetate (2 X 200ml_), washed with brine (100ml_) then concentrated to provide the title compound as a white solid. (17 g, 67.9 mmol, 88% yield). LCMS m/z 248.2 (M+H)+,1.678min (ret.time).

The synthetic route of 2854-16-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ASTEX THERAPEUTICS LIMITED; COOPER, Anthony William James; GOODWIN, Nicole Cathleen; GRIFFITHS-JONES, Charlotte Mary; HEIGHTMAN, Thomas Daniel; KERNS, Jeffrey K.; WILLEMS, Hendrika Maria Gerarda; YAN, Hongxing; (215 pag.)WO2018/109649; (2018); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Electric Literature of 41175-50-2 ,Some common heterocyclic compound, 41175-50-2, molecular formula is C12H15NO, 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.

/V-ethyl-/V-(2,3,6,7-tetrahydro-1 H,5H,12H-quinolizino[1,9-bc]phenoxazin-12- ylidene)ethanaminium (LGW-02-86). Compound 26 (50 mg, 0.26 mmol) was dissolved in a solution of /-PrOH/H20 (9/1 , 1 mL) at 80 C for 30 min. A suspended solution of 35 (58 mg, 0.28 mmol) and HCICU (70%, 30 mI_) in 90% /-PrOH (2 ml_) was added in 4 portions over 1 h. The resulting solution was stirred overnight. After which, the dark blue solution was evaporated under reduced pressure, and the residue was purified on a Biotage Isolera Flash System using SNAP Ultra cartridge with a mobile phase of CHCI3 and MeOH containing 0.5% formic acid (gradient, 2-15% of MeOH in CHCI3). The fractions containing product were pooled and evaporated, affording LGW-02-86 (36 mg, 34%) as a dark blue solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,41175-50-2, its application will become more common.

Reference:
Patent; OREGON HEALTH & SCIENCE UNIVERSITY; OREGON STATE UNIVERSITY; GIBBS, Summer L.; BARTH, Connor W.; ALANI, Wathah G.; SHAH, Vidhiben; WANG, Lei; (167 pag.)WO2020/33435; (2020); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts