Month: November 2020

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 78573-45-2, name is 3-(3-(Trifluoromethyl)phenyl)propan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. 78573-45-2

Step 3: Preparation of Compound III (i.e., 3-(3-trifluoromethylphenyl)propanal) To a solution of 10 g (48 mmol) of Compound VII, 76.6 mg of TEMPO (2,2,6,6-tetramethyl-1-piperidinyloxy free radical) and 234 mg of potassium bromide in 70 mL methylene chloride was added 220 mL (pH=9.5) of sodium hypochlorite solution over 20 minutes at 10-15 C. with stirring. After five minutes of additional stirring, the organic layer was separated. The aqueous layer was extracted twice with 40 mL of methylene chloride, and the collected organic layers were dried and evaporated to yield 10 g of crude Compound III as a yellowish liquid. Yield: 100%; purity (determined by GC): 90.3%, contains 8.25% of Compound NMR data (200 MHz, CDCl3, ppm): 2.81 (t, 2H), 3.00 (t, 21-1), 7.37-7.46 (m, 4H), 9.80 (s, 1H).

Statistics shows that 78573-45-2 is playing an increasingly important role. we look forward to future research findings about 3-(3-(Trifluoromethyl)phenyl)propan-1-ol.

Reference:
Patent; Medichem, S.A.; US2010/267988; (2010); A1;,
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647-42-7, A common compound: 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol,molecular formula is C8H5F13O, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

Into a 2 L four-necked flask equipped with a stirrer, a thermometer and a cooling tube,800 g (2.2 mol) of FA-6 (manufactured by Unimartech) and 175.78 g (4.4 mol) of granular NaOH (manufactured by Wako Pure Chemical Industries, Ltd.) were added. Under a nitrogen atmosphere, while stirring at 200 rpm with a Teflon (registered trademark) 12 cm crescent stirring blade, the temperature was heated to 60 C. in the flask.398.73 g (3.3 mol) of allyl bromide (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise thereto over 2 hours. After completion of the dropwise addition, the mixture was stirred at 70 C. for 1 hour and at 80 C. for 1 hour.Thereafter, the temperature was raised to 130 C. to remove excess allyl bromide.After cooling to 60 C., 800 g of ion-exchanged water was added, stirred for 30 minutes, then allowed to stand to separate the layers.The upper aqueous layer was withdrawn, 800 g of ion-exchanged water was added, and the mixture was stirred again, allowed to stand still and the aqueous layer was removed. Dehydrated at 60 C./5 KPa and distilled at 100 C./2 KPa to obtain 774.9 g of C 6 F 13 –CH 2 CH 2 –O – CH 2 CHCH 2 (yield 88%) as a fraction.

With the rapid development of chemical substances, we look forward to future research findings about 647-42-7.

Reference:
Patent; KAO CORP; ??????; IIDA MASAYUKI; Iida Masayuki; SHINBO AYUMI; Susumu Kuni Ayumi; (15 pag.)JP2016/121094; (2016); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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. 111-90-0, name is Diethylene Glycol Monoethyl Ether. A new synthetic method of this compound is introduced below., 111-90-0

Diethylene glycol monoethyl ether (1 equiv.) and water (1 mL) were mixed together and stirred on ice before addition of NaOH (2.95 equiv.) and 0.4 M tetrabutylammonium hydroxide (aq) (0.05 equiv.). Once the mixture returned to 0C, epichlorohydrin (2.95 equiv.) was added portion-wise over 3 mm. The mixture was stirred at room temperature for 16 hours. H20 (15 mL) was added and the mixture was extracted with EtOAc (4x 30 mL). The combined extracts were washed with brine (30 mL) and dried over Na2SO4. The extracts were concentrated under reduced pressure. The residue was distilled under vacuum, providing a as a colorless liquid boiling at 110-117C (0.1 mmHg).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,111-90-0, Diethylene Glycol Monoethyl Ether, and friends who are interested can also refer to it.

Reference:
Patent; CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE; UNIVERSITE DE BORDEAUX; INSTITUT POLYTECHNIQUE DE BORDEAUX; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; LECOMMANDOUX, Sebastien, Jean, Marie; GARANGER, Elisabeth, Beatrice, Michele; DEMING, Timothy; (40 pag.)WO2017/21334; (2017); A1;,
Alcohol – Wikipedia,
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13826-35-2, 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. 13826-35-2, name is (3-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.

General procedure: To an oven-dried 20 cm3 test tube with a ground-in stopperequipped with a stir bar were added anthranilamide (1.0 mmol), benzyl alcohol (1.0 mmol), KOH (2.0 mmol),and 4 cm3 toluene. The test tube was put in an oil bath potpreheated at 90 C and the mixture was stirred for 20 h at90 C. After cooling to room temperature, the reactionmixture was added about 5 g silica gel and directly condensedon a rotator under vacuum. The resulting residualwas transferred to a silica gel chromatography column andeluted with a solution of petroleum ether and ethyl acetate[4/1 (v/v)] to give a white solid 2-phenyl-4(3H)-quinazolinone.For some products (3f, 3g, 3n, and 3t) onlysparingly soluble in ethyl acetate, the reaction mixtureswere condensed in vacuo on a rotary evaporator. Theresiduals were washed three times with water and oncewith ethyl acetate, and then dried in an infrared oven togive the desired products pure enough for NMR analysis.

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. 13826-35-2, (3-Phenoxyphenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Qiu, Dezhi; Wang, Yanyan; Lu, Dongming; Zhou, Lihong; Zeng, Qingle; Monatshefte fur Chemie; vol. 146; 8; (2015); p. 1343 – 1347;,
Alcohol – Wikipedia,
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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. 870-72-4, name is Hydroxymethanesulfonic Acid Sodium Salt, the common compound, a new synthetic route is introduced below. 870-72-4

3, 9-Bis (sodium methylenesulfonato)-3, 6, 9, 15-tetraazabicyclo [9. 3. IJpentadeca- 1(15),11,13-triene (10). 3,6, 9, 15-tetraazabicyclo- [9. 3. 1] pentadeca-1 (15), 11, 13-triene (PYCLEN) (8) (2 g, 9.7 mmol) was dissolved in 20 ml water and the pH was adjusted to 5 using 6N HCl. The sodium formaldehyde bisulfite (9) (2.65g, 19.77 mmol) was then added in one portion and the pH was maintained at 7.0 using IN KOH. When no further drop in pH was detected, the pH was raised to 8.5 followed by freeze-drying to give the product as a white solid(quantitative). 1H NMR (D2O)8 2.87 (t, -CH2-, 5,7-cyclic, J H-H = 5.2 Hz, 4 H), 3.18 (t, -CH2-, 4, 8-cyclic, JH-H= 5. 2 Hz, 4 H), 3.85 (s, -CH2-, 2,10- cyclic, 4 H), 4.11 (s, N-CH2-S, 4 H), 7.03 (d, 3,5-py, JH-H = 7.7 Hz, 2 H), 7.55 (t, 4-py, J H-H = 7.7 Hz, 1 H); 13 C {1H} NMR(D20) 6 48.52 (-CH2-, 5,7-cyclic), 54.04 (-CH2-, 4,8- cyclic), 58.92 (-CH2-, 2,10-cyclic), 75.09 (N-CH2-S), 123.90 (3,5-py), 141.37 (4-py), 161.89 (2,6-py).

Statistics shows that 870-72-4 is playing an increasingly important role. we look forward to future research findings about Hydroxymethanesulfonic Acid Sodium Salt.

Reference:
Patent; DOW GLOBAL TECHNOLOGIES INC.; WO2005/49096; (2005); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding some certain compound to certain chemical reactions, such as: 124-68-5, name is 2-Amino-2-methyl-1-propanol, 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 124-68-5. 124-68-5

1-a. A mixture of 2-amino-2-methyl-1-propanol (53 g), di-t-butyl dicarbonate (65 g) and water (500 ml) was stirred at room temperature for 1 hour. The reaction mixture was extracted with chloroform, and the chloroform layer was dried over MgSO4. The solvent was evaporated under reduced pressure. The residue was recrystallized from hexane to give 2-(t-butoxycarbonylamino)-2-methyl-1-propanol (44.4 g). NMR (CDCl3)delta: 1.25 (6H, singlet), 1.43 (9H, singlet), 3.20-5.50 (2H, multiplet), 3.56 (2H, singlet).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 124-68-5.

Reference:
Patent; Teikoku Hormone Mfg. Co., Ltd.; US4843072; (1989); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

702-82-9, Adding a certain compound to certain chemical reactions, such as: 702-82-9, 3-Aminoadamantan-1-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, 702-82-9, blongs to alcohols-buliding-blocks compound.

Example-17: Preparation of 2-(3-hydroxyadamantan-l-yl-imino) acetic acid compound of formula 11:To the solution of l-aminoadamantane-3-ol (5 grams) in 50 ml of tetrahydrofuran 2-oxo acetic acid (2.25 grams) was added and stirred. The reaction mixture was heated to reflux for 3 hrs. The reaction mixture was cooled to room temperature and quenched with water. The reaction mixture was extracted with dichloromethane. The dichloromethane solvent was dried and distilled off to get the title compound.Yield: 6 grams.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,702-82-9, its application will become more common.

Reference:
Patent; MSN LABORATORIES LIMITED; SATYANARAYANA REDDY, Manne; ESWARAIAH, Sajja; VENKAT REDDY, Ghojala; KONDAL REDDY, Bairy; WO2011/101861; (2011); A1;,
Alcohol – Wikipedia,
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702-82-9, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 702-82-9, name is 3-Aminoadamantan-1-ol. This compound has unique chemical properties. The synthetic route is as follows.

Example 1 : Preparation of vildagliptin To the (S)-l-(2-chloroacetyl)pyrrolidine-2-carbonitrile (100 gm) was added FontWeight=”Bold” FontSize=”10″ isopropyl acetate (400 ml) and dimethylformamide (400 ml) at room temperature and then heated to 40C for 15 minutes to provide a solution. A mixture of 3-hydroxy-l- aminoadamantane (100 gm), 2-butanone (700 ml), potassium iodide (5 gm) and potassium carbonate (400 gm) were added to the solution. The reaction mixture was maintained for 1 hour at room temperature and then heated to 75 to 80C. The reaction mass was maintained for 1 hour at 75 to 80C, filtered and then concentrated to provide a residual solid. To the residual solid was added a mixture of diisopropyl ether (900 ml) and isopropyl acetate (100 ml) and then heated to 70C. The reaction mass was then cooled to room temperature and further cooled to 0 to 5C. The contents were maintained for 1 hour at room temperature and filtered. The solid thus obtained was dried to provide 100 gm of vildagliptin.

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 702-82-9, 3-Aminoadamantan-1-ol.

Reference:
Patent; HETERO RESEARCH FOUNDATION; PARTHASARADHI REDDY, Bandi; RATHNAKAR REDDY, Kura; MURALIDHARA REDDY, Dasari; SUBASH CHANDER REDDY, Kesireddy; VAMSI KRISHNA, Bandi; WO2014/13505; (2014); A2;,
Alcohol – Wikipedia,
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558-42-9, 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. 558-42-9, name is 1-Chloro-2-methyl-2-propanol, molecular formula is C4H9ClO, 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.

[0157] 7-Iodo-2H-pyrazolo[4,3-b]pyridine (300 mg, 1.224 mmol), l-chloro-2-methylpropan- 2-ol (133 mg, 1.224 mmol) and CS2CO3 (399 mg, 1.224 mmol) were combined in DMF (5 mL). The mixture was heated at 120 ¡ãC for 30 minutes using a microwave. The reaction mixture was then purified by preparative HPLC using a Sunfire Prep 5muiotaeta CI 8, 75 X 30 mm column eluting with a gradient of 05 – 25percent acetonitrile (containing 0.035percent TFA) in water (containing 0.05percent> TFA) using basic buffer to afford l-(7-iodo-2H-pyrazolo[4,3-b]pyridin- 2-yl)-2-methylpropan-2-ol (170 mg, 0.536 mmol, 43.8 percent yield). MS [M+H] found 318.

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. 558-42-9, 1-Chloro-2-methyl-2-propanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; KWOK, Lily; LARSON, John David; SABAT, Mark; WO2011/146287; (2011); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

2050-25-1 , The common heterocyclic compound, 2050-25-1, name is 2-(2-(Benzyloxy)ethoxy)ethanol, molecular formula is C11H16O3, 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 (i): 2-(2-(Benzyloxy)ethoxy)ethyl methanesulfonate (47) MsCI (15.8 mL. 204 mmol) was added to a solution of 2-(2-(benzyloxy)ethoxy)ethanol (46) (25 g, 127 mmol) and Et3N (36 mL, 255 mmol) in DCM (180 mL) at 0C, the reaction mixture was allowed to warm up to RT and stirred for 16h. The reaction mixture was diluted with DCM (50 mL) and washed with water (2 x 50 mL), 1 M HCI (aq.) (2 x 50 mL), the organic layer was dried (MgS04), filtered and concentrated in vacuo to afford 2-(2-(benzyloxy)ethoxy)ethyl methanesulfonate (47) (35 g, 100 %) as an orange oil: m/z 275 (M+H)+ (ES+). 1 H NMR (400 MHz, CDCIs) delta: 7.37-7.27 (m, 5H), 4.55 (s, 2H), 4.40-4.37 (m, 2H), 3.78-3.76 (m, 2H), 3.71-3.68 (m, 2H), 3.64-3.62 (m, 2H), 3.02 (s, 3H).

According to the analysis of related databases, 2050-25-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; UNIVERSITY OF LEICESTER; ANDREW, Peter William; LONNEN, Rana; DAMASO, Mafalda Pires; FRICKEL, Fritz-Frieder; HIRST, Simon Christopher; DAVIES, Mark William; HAMZA, Daniel; WO2013/83975; (2013); A2;,
Alcohol – Wikipedia,
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