Month: June 2021

Application of 431-38-9, 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. 431-38-9, name is 3-Amino-1,1,1-trifluoropropan-2-ol, molecular formula is C3H6F3NO, 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.

6-(4-Ch lorophenyl)-3-oxo-2-(pyridin-3-yl)-2 ,3-d ihyd ropyridazine-4-carboxylic acid (100 mg,0.31 mmol) was dissolved in anhydrous DMF (2.3 mL). (2RS)-3-Amino-1,1,1-trifluoropropan-2-ol (78.8 mg, 0.61 mmol), N-ethyl-N-isopropylpropan-2-amine (0.239 mL, 1.37 mmol), and propane phosphonic acid anhydride (T3P, 267 pL, 50% in DMF, 458 pmol) were successively added. It was stirred at rt overnight. The crude reaction mixture was purified by RP-HPLC (column: X-Bridge 018 5pm lOOx3Omm, mobile phase: (water + 0.2 vol% aqueous ammonia (32%)) acetonitrile, gradient) to yield 23 mg (23%) of the title compound.1H-NMR (400MHz, DMSO-d6): 6 [ppm] = 3.43 -3.52 (m, 1H), 3.71 -3.79 (m, 1H), 4.17-4.28(m, 1H), 6.66 (d, 1H), 7.57 -7.61 (m, 2H), 7.64 (dd, 1H), 7.99 -8.04 (m, 2H), 8.17 (ddd, 1H),8.66 – 8.73 (m, 2H), 8.92 (br s, 1 H), 9.61 (t, 1 H).

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 431-38-9, 3-Amino-1,1,1-trifluoropropan-2-ol.

Reference:
Patent; BAYER AKTIENGESELLSCHAFT; BAYER PHARMA AKTIENGESELLSCHAFT; DEUTSCHES KREBSFORSCHUNGSZENTRUM; GUTCHER, Ilona; ROeHN, Ulrike; SCHMEES, Norbert; ZORN, Ludwig; ROeSE, Lars; BADER, Benjamin; KOBER, Christina; CARRETERO, Rafael; STOeCKIGT, Detlef; IRLBACHER, Horst; PLATTEN, Michael; (397 pag.)WO2018/146010; (2018); A1;,
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Electric Literature of 456-47-3, 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. 456-47-3, name is 3-Fluorobenzyl alcohol, molecular formula is C7H7FO, 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.

The oxidation of alcohols was carried out under O2 in a 50-mL two-necked, round-bottom flask equipped with a magnetic stirrer. Typically, Fe2(SO4)3 (0.25 mmol) and TMHPO (0.25 mmol) were added to the flask, followed by 15 mL of a CH3CN/H2O (1:2) solvent mixture. After stirring for 5 min, the alcohol (5 mmol) was added, followed by NaNO2 (0.25 mmol). The resulting mixture was stirred at room temperature and 1 atm pressure of oxygen. When the reactions were completed, the reaction mixture was transferred to a separating funnel and extracted with dichloromethane. The organic layer was dried over anhydrous Na2SO4 and concentrated and further purified by flash chromatography to give the desired product.

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 456-47-3, 3-Fluorobenzyl alcohol.

Reference:
Article; Shi, Xiang-Jun; Qian, Jie; Tan, Fan-Fan; Yu, Chuan-Ming; Journal of Chemical Research; vol. 37; 7; (2013); p. 398 – 401;,
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Related Products of 13674-16-3 , The common heterocyclic compound, 13674-16-3, name is Methyl 2-hydroxy-3-phenylpropanoate, molecular formula is C10H12O3, 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.

The compound 5-hydroxy-6-nitro-1H-indazole-1-carboxylic acid tert-butyl ester (900 mg, 3.22 mmol), methyl 2-hydroxy-3-phenylpropionate (870 mg, 4.83 mmol) and triphenylphosphine (1.69g, 6.44mmol) was dissolved in dry THF (80mL) was added DIAD (1.3g, 6.44mmol) at 0 C, Stirrer at room temperature until the starting material is completely reacted.The solvent was spin dried, ethyl acetate (200mL * 3). The combined organic phases were dried, filtered, concentrated to give pale yellow solid product 5-((1-methoxy-1-carbonyl-3-phenylpropan-2-yl)oxo)-6-nitro-1H-indazole-1-carboxylic acid tert-butyl ester (1.4 g, yield 98%)

The synthetic route of 13674-16-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanghai Hansen Bio-pharmaceutical Technology Co., Ltd.; Jiangsu Haosen Pharmaceutical Group Co., Ltd.; Liu Shiqiang; Zhou Yuanfeng; Bao Meng; Yuan Yida; Liu Lei; Bao Rudi; (57 pag.)CN109761986; (2019); A;,
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Adding a certain compound to certain chemical reactions, such as: 101597-25-5, 1,1-Bis(4-methoxyphenyl)prop-2-yn-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, name: 1,1-Bis(4-methoxyphenyl)prop-2-yn-1-ol, blongs to alcohols-buliding-blocks compound. name: 1,1-Bis(4-methoxyphenyl)prop-2-yn-1-ol

General procedure: To a refluxing solution of 5-hydroxy-3-methoxy-7H-benzo[c]fluoren-7-one 12-4 (3.00 g, 10.9 mmol) in a mixture of toluene (123 mL) and 2-butanone (45 mL) were added 1,1-bis(4-methoxyphenyl)propyn-1-ol (5.23 g, 19.5 mmol) and catalytic amount of p-TsOH, and the resulting mixture was refluxed for 30 min. The solution was cooled down to room temperature, then 10% aq. sodium hydroxide (21 mL), tetrahydrofuran (120 mL) and10% aq. sodium chloride were added and the mixture was stirred well. The organic layer was separated, washed with water four times, and the solvent removed in vacuo. To the resulting residue was added acetone (100 mL) and the mixture was refluxed for 1 h. After the mixture was cooled down, the solid material precipitated was collected by filtration. After drying in vacuo, 6-methoxy-3,3-bis(4-methoxyphenyl)benzo[3,4]fluoreno[2,1-b]pyran-13(3H)-one 13-7 was obtained as a dark purple solid (2.47 g, 4.70 mmol) in 43% yield. 13-7: Mp 207-209 C. 1H NMR (CDCl3) delta/ppm 3.77 (3H, s), 3.96 (3H, s), 6.27 (1H, d, J = 10.0 Hz), 6.84 (4H, m), 7.20 (2H, m), 7.40 (5H, m), 7.57 (2H, m), 7.80 (1H, d, J = 8.0 Hz), 7.86 (1H, d, J = 10.0 Hz), 8.27 (1H, d, J = 9.2 Hz). LC-MS 527.2033 (M+1) (Calculated exact mass for C35H27O5 (M+1) 527.1853). FT-IR (KBr) nu/cm-1 3014, 2953, 2831, 1695, 1605, 1505, 1466, 1397, 1373, 1277, 1218.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,101597-25-5, 1,1-Bis(4-methoxyphenyl)prop-2-yn-1-ol, and friends who are interested can also refer to it.

Reference:
Article; Momoda, Junji; Izumi, Shinobu; Yokoyama, Yasushi; Dyes and Pigments; vol. 119; (2015); p. 95 – 107;,
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Application of 495-76-1, 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 495-76-1 as follows.

5-(Bromomethyl)-1,3-benzodioxole was prepared using reportedmethod [30]. Take a 250 ml round bottom flask A charged with 1,3-benzodioxole-5-methanol (5 g; 32.86 mmol) in dry diethyl ether(50 ml). Take another 100 ml round bottom flask B loaded with 3.1 ml(32.86 mmol; 1 equiv.) of phosphorous tribromide dissolved in 40 mlof diethyl ether. A dropwise addition was carried out from flask B toflask A maintaining the temperature at 0 C for and stirred for 15 min.After the completion of the reaction, the reaction mixture was workedupwithwater (3× 100ml) using a separating funnel followed bywashingwith brine (1:1). After drying over sodium sulphate and filtration,the solvent was evaporated on a vacuum rotary evaporator. The crudewas recrystallized in petroleum ether to get the desired white solidproduct.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,495-76-1, its application will become more common.

Reference:
Article; Sehrawat, Hitesh; Kumar, Neeraj; Tomar, Ravi; Kumar, Loveneesh; Tomar, Vartika; Madan, Jitender; Dass, Sujata K.; Chandra, Ramesh; Journal of Molecular Liquids; vol. 302; (2020);,
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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.111-90-0, name is Diethylene Glycol Monoethyl Ether, molecular formula is C6H14O3, molecular weight is 134.1736, as common compound, the synthetic route is as follows.name: Diethylene Glycol Monoethyl Ether

Example Al 4; a. Preparation of intermediate 38; NaH (60 % in oil; 0.0072 mol) was added portionwise at 0 C to a solution of 2-(2- ethoxyethoxy)-ethanol (0.0072 mol) in THF (12.5 ml) under N2 flow. The mixture was stirred at 0C for 1 hour. A solution of intermediate 10 (0.006 mol) in THF (12.5 ml) was added dropwise. The mixture was stirred and refluxed for 18 hours and was then cooled to room temperature. EtOAc and H2O were added. The organic layer was washed with H2O and then with saturated NaCl. The separated organic layer was dried (MgSO4), filtered and the solvent was evaporated. Yield: 2.5 g intermediate 38 (97 %). EPO

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; JANSSEN PHARMACEUTICA N.V.; WO2007/436; (2007); A1;,
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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. 873-76-7, name is (4-Chlorophenyl)methanol, molecular formula is C7H7ClO, 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. category: alcohols-buliding-blocks

General procedure: To a 25-mL Schlenk tube equipped with a magnetic stirrer, CuCl (0.05 mol, 5 mol%), DABCO (0.10 mol, 10 mol%), 4-HO-TEMPO (0.05 mmol, 5 mol%) were added. Substrates 1 (1 mmol) and NH3 (aq, 25-28%, 3 mmol, 3.0 equiv) in CH3CN (2 mL) were added subsequently. Then the reaction mixture was stirred at room temperature for 24 h in the presence of an air balloon. The progress of the reaction was monitored by TLC. After completion, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was dried over anhydrous MgSO4. Subsequently, the combined organic layer was concentrated under reduced pressure and the crude product was purified by column chromatography to afford the corresponding products

With the rapid development of chemical substances, we look forward to future research findings about 873-76-7.

Reference:
Article; Hu, Yongke; Chen, Lei; Li, Bindong; Chinese Chemical Letters; vol. 29; 3; (2018); p. 464 – 466;,
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Application of 60666-70-8, Adding some certain compound to certain chemical reactions, such as: 60666-70-8, name is (2-Bromo-5-chlorophenyl)methanol,molecular formula is C7H6BrClO, 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 60666-70-8.

Add compound 3 (500 mg, 2.26 mmol) in DCM (40 mL) and DIPEA (1.12 mL, 6.77 mmol)DMAP (55.16 mg, 451.51 mumol) was added. Then, pivaloyl chloride (416.65 uL, 3.39 mmol) was added dropwise at 0 ° C to react.The mixture was stirred at 10 ° C for 0.1 hour and then at room temperature overnight. The reaction mixture was diluted with DCM and then usedWater, 10percent citric acid and brine were washed with MgSO4 and filtered. The filtrate was concentrated to give a crude product which was purified by CC.The compound 4 (605 mg, 87.69percent) was obtained as a pale yellow oil.

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. 60666-70-8, (2-Bromo-5-chlorophenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Chinese Academy Of Sciences Tianjin Industry Bio-technology Institute; Lin Jianping; Liu Pi; Li Jinlong; Wang Zhonghua; Liu Cui; (15 pag.)CN108264467; (2018); A;,
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Application of 10160-28-8 ,Some common heterocyclic compound, 10160-28-8, molecular formula is C9H16O, 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.

To a mixture of non-8-yn-1-ol (5.00 g, 35.6 mmol, CAS10160-28-8) and TEA (10.8 g, 106 mmol, 14.8 mL) in DCM (100 mL) was added MsCl (6.13 g, 53.4 mmol, 4.14 mL). The reaction mixture was stirred at 25 C. for 2 hours. On completion, the reaction mixture was concentrated in vacuo. The residue was diluted with water (10 mL) and extracted with DCM (3×10 mL). The combined organic layers was dried over Na2SO4, filtered and concentrated in vacuo to give the title compound (7.70 g, 98% yield) as light yellow oil. 1H NMR (400 MHz, CDCl3) delta 4.23 (t, J=6.4 Hz, 2H), 3.01 (s, 3H), 2.22-2.18 (m, 2H), 1.95 (t, J=2.4 Hz, 1H), 1.80-1.73 (m, 2H), 1.58-1.50 (m, 2H), 1.47-1.36 (m, 6H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,10160-28-8, its application will become more common.

Reference:
Patent; Kymera Therapeutics, Inc.; Mainolfi, Nello; Ji, Nan; Kluge, Arthur F.; Weiss, Matthew M.; Zhang, Yi; (1443 pag.)US2019/192668; (2019); A1;,
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Adding a certain compound to certain chemical reactions, such as: 10160-24-4, 7-Bromo-1-heptanol, 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, Application In Synthesis of 7-Bromo-1-heptanol, blongs to alcohols-buliding-blocks compound. Application In Synthesis of 7-Bromo-1-heptanol

To a stirred solution of (S)-3- (1-CARBAMOYL-1,1-DIPHENYLMETHYL)pyrrolidine (40 g, 142.7 mmol) and triethylamine (59.6 mL, 428 mmol) in acetonitrile (1. 1 L) at 40C under a nitrogen atmosphere was added 7-bromo-1-heptanol (24 mL, 146 mmol) in acetonitrile (100 mL) dropwise. The reaction mixture was heated to 50C for 9 hours. The reaction mixture was allowed to cool before removing the solvent under reduced pressure. The crude residue was dissolved in dichloromethane (500 mL) and the organic layer washed with saturated aqueous sodium bicarbonate (2 x 300 mL), followed by water (300 mL) and saturated aqueous sodium chloride (300 mL), and then dried over magnesium sulfate (10 g). The magnesium sulfate was filtered off and washed with dichloromethane (100 mL). The solvent was then removed in vacuo to give the crude product which was purified on a short column (SIO2) by varying the eluant from 19: 1: 0.1 to 3: 1: 0.1 CH2CL2/MEOH/NH40H to give 31.35 g of the title intermediate as a white solid (56% yield ; >95% purity by HPLC Method A).

The synthetic route of 10160-24-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; THERAVANCE, INC.; WO2004/41806; (2004); A2;,
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