Tag: M.W=0-100

2854-16-2, 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.2854-16-2, name is 1-Amino-2-methylpropan-2-ol, molecular formula is C4H11NO, molecular weight is 89.14, as common compound, the synthetic route is as follows.

j0086J To a 15 L glass reactor purged with nitrogen was charged Compound 14 (1.038 kg, 2.47 mol, 1 eq), followed by Me-THF (6.176 kg) and DIEA (0.384 kg, 2.97 mol, 1.2 eq). The resulting mixture was stirred at room temperature and then 1-amino-2-methylpropan-2-ol(0.265 kg, 2.97 mol, 1.2 eq) in Me-THF (2.647 kg) was slowly charged while maintaining 20-30 ¡ãC. After the reaction was complete, water (2.6 L) and n-heptane (2.076 kg) were added. The mixture was stirred for 20 mm., the aqueous layer was removed, water (2.6 L) was added and the pH of the aqueous phase adjusted to 7 using 0.1N HC1. The aqueous layer was removed, and the organic layer was washed with water (2 x 2.6 L), 4percent NaHCO3 (1.1 L), and water (1.15 L). The organic layer was concentrated under vacuum to 3.4 L. Me-THF (4.950 kg) was added, and the mixture was concentrated to 3.4 L. The residue was diluted with Me-THF (4.931 kg). The solution was clarified through a 1.2 t in-line filter. The clarified solution was concentrated to 2.6 L. The residue was heated to 45 ¡ãC, and then n-heptane (2.599 kg) was added slowly while maintaining 45 ¡ãC. The batch was seeded with 2-methyl-i -((4-(6-(trifluoromethyl)pyridin-2-yl)- 6-((2-(trifluoromethyl)pyridin-4-yl)amino)- 1,3,5 -triazin-2-yl)amino)propan-2-ol (lOg). nHeptane (2.599 kg) was added slowly while maintaining 45 ¡ãC. After ih, the batch was cooled down to 20 ¡ãC. The mixture was stirred at 20 C for ih. The batch was filtered. The solids were washed with n-heptane (2 x 1 L), and then vacuum-dried at 35 ¡ãC in an oven for 20 h. Isolated yield: 1.124 kg of 2-methyl-i -((4-(6-(trifluoromethyl)pyridin-2-yl)-6-((2- (trifluoromethyl)pyridin-4-yl)amino)- 1,3,5 -triazin-2-yl)amino)propan-2-ol (96 percent) as a light yellow powder.

Statistics shows that 2854-16-2 is playing an increasingly important role. we look forward to future research findings about 1-Amino-2-methylpropan-2-ol.

Reference:
Patent; AGIOS PHARMACEUTICALS, INC.; ZHANG, Shijie; (47 pag.)WO2017/24134; (2017); A1;,
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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 56-81-5 as follows., 56-81-5

4.2.7 cis-2-Phenyl-1,3-dioxan-5-ol (18) Concentrated sulfuric acid (3 drops) was added to a mixture of glycerol (44 mL, 55 g, 0.60 mol) and freshly distilled benzaldehyde (48 mL, 50 g, 0.47 mol) in toluene (69 mL). The resulting mixture was heated to reflux in a Dean-Stark water separator. When the separation of water was complete (8.5 mL), the reaction mixture was allowed to cool to room temperature and the solvent removed in vacuo. The resulting white solid was recrystallized from isopropyl ether/petroleum ether. The precipitate was filtered off and purified by flash column chromatography (? = 6 cm, h = 15 cm, V = 50 mL, cyclohexane/ethyl acetate = 2:1, Rf = 0.16) to give 18 as colorless solid (42.6 g, 0.24 mol, 50% yield). Mp = 81 C; 1H NMR (DMSO-d6): delta [ppm] = 3.48-3.52 (m, 1H, OCH2CHOH), 3.91-3.97 (m, 2H, OCH2CHOH), 4.01-4.07 (m, 2H, OCH2CHOH), 4.99 (d, J = 4.8 Hz, 1H, OH), 5.53 (s, 1H, CHPh), 7.33-7.40 (m, 3H, 3′-Hphenyl, 4′-Hphenyl, 5′-Hphenyl), 7.42-7.47 (m, 2H, 2′-Hphenyl, 6′-Hphenyl); 13C NMR (DMSO-d6): delta [ppm] = 62.4 (1C, OCH2CHOH), 71.4 (2C, OCH2CHOH), 100.2 (1C, CHPh), 126.2 (2C, C-2’phenyl, C-6’phenyl), 127.9 (2C, C-3’phenyl, C-5’phenyl), 128.5 (1C, C-4’phenyl), 138.9 (1C, C-1’phenyl); IR (neat): [cm-1] = 3271, 2916, 2851, 1450, 1385, 1339, 1277, 1153, 1084, 995, 976, 806, 741, 694; HRMS (m/z): [M+H]+ calcd for C10H13O3, 181.0859; found, 181.0878; HPLC (method 1): tR = 11.7 min, purity 95.4%.

The chemical industry reduces the impact on the environment during synthesis 56-81-5, I believe this compound will play a more active role in future production and life.

Reference:
Article; Tangherlini, Giovanni; Torregrossa, Tullio; Agoglitta, Oriana; Koehler, Jens; Melesina, Jelena; Sippl, Wolfgang; Holl, Ralph; Bioorganic and Medicinal Chemistry; vol. 24; 5; (2016); p. 1032 – 1044;,
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124-68-5, 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. 124-68-5, name is 2-Amino-2-methyl-1-propanol. A new synthetic method of this compound is introduced below.

2-Amino-2-methylpropan-l-ol (5g, 89.13 mmol) was reacted with benzyl chloroformate (8.61 g, 50.5 mmol), using triethylamine (7.38 g, 72.9 mmol) as base in DCM solvent (50mL) at room temperature for 3 hours. After completion of the reaction, the organic layer was washed with water (2 x 20 mL) and dried over sodium sulfate. The DCM layer upon concentration under vaccum afforded benzyl (l-hydroxy-2-methylpropan-2- yl)carbamate (Compound 7b).

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. 124-68-5, 2-Amino-2-methyl-1-propanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NEKTAR THERAPEUTICS (INDIA) PVT. LTD.; NEKTAR THERAPEUTICS; SHARMA, PANKAJ; KHATRI, VIJAY KUMAR; GU, XUYUAN; SONG, YUAN; SHEN, MICHAEL LIXIN; SAUTHIER, JENNIFER RIGGS; ANAND, NEEL K.; KOZLOWSKI, ANTONI; ODINECS, ALEKSANDRS; RILEY, TIMOTHY A.; REN, ZHONGXU; MU. YONGQI; SHEN, XIAOMING; YUAN. XUEJUN; AURRECOECHEA, NATALIA; O’MAHONY, DONOGH JOHN ROGER; WO2015/92819; (2015); A2;,
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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. 764-48-7, name is Ethylene Glycol Vinyl Ether. This compound has unique chemical properties. The synthetic route is as follows. 764-48-7

General procedure: A dry and argon-flushed 10 mL Schlenk tube, equipped with a stirring bar and septum, wascharged with 2-(vinyloxy)ethanol (5, 132 mg, 1.50 mmol, 1.50 equiv) in Et2O (1.5 mL). Then,iPrMgBr (1.55 mmol, 1.55 equiv) was added dropwise at 25 C. After 5 min of stirring,Sc(OTf)3 (49.2 mg, 0.10 mmol, 0.10 equiv) and aldehyde 6 (1.00 mmol, 1.00 equiv) weresuccessively added and the reaction mixture was stirred at 40 C for the given time. After afull conversion was detected by GC-analysis, sat. aq. NH4Cl (15 mL) was added and theaqueous layer was extracted with EtOAc (3 x 15 mL). The combined organic layers weredried over Na2SO4, filtered and solvent was removed under reduced pressure. Purification viacolumn chromatography (SiO2) afforded expected products 4.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 764-48-7, Ethylene Glycol Vinyl Ether.

Reference:
Article; Quinio, Pauline; Kohout, Laura; Roman, Daniela Sustac; Gaar, Jakob; Karaghiosoff, Konstantin; Knochel, Paul; Synlett; vol. 27; 11; (2016); p. 1715 – 1719;,
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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 2854-16-2, name is 1-Amino-2-methylpropan-2-ol. This compound has unique chemical properties. The synthetic route is as follows. 2854-16-2

5-(2 ,4-dichloro-5-(3-fluoropyridin-2-yl)benzamido)- 1 -phenyl- 1 H-pyrazole-3-carboxylicacid (Example 107, 78 g, 166 mmol) was sonicated in DMF (300 mL) with N,Ndiisopropylethylamine (58 mL, 332 mmol) to give a clear solution, which was cooled to 10CC. TPTU (74 g, 249 mmol) was added portionwise and the mixture stirred at 10C for20 minutes. A solution of 1-amino-2-methylpropan-2-ol (22.1 g, 249 mmol) in DMF (50 mL) was added dropwise at 1000 and the mixture then allowed to warm to room temperature and stirred for 16 hours. The reaction mixture was partitioned between EtOAc (600 mL) and water (600 mL). The aqueous layer was separated and extracted with additional EtOAc (3 x 200 mL). The combined organic layers were washed withsaturated aqueous ammonium chloride solution (300 mL), water (5 x 200 mL), dried (magnesium sulphate) and concentrated in vacuo to give an orange oil. The oil was treated with acetonitrile (300 mL) and the resulting solid collected by filtration, washed with acetonitrile and dried under vacuum to afford the title compound as a colourless solid (60 g, 66%).1H NMR (400MHz, DMSO-d6): O ppm 1.09 (s, 6H), 3.21-3.22 (d, 2H), 4.63 (5, 1H), 6.93(5, 1H), 7.45-7.49 (m, 1H), 7.50-7.55 (t, 2H), 7.58-7.65 (m, 3H), 7.69 (5, 1H), 7.80-7.85(t, 1H), 7.87-7.95 (m, 2H), 8.56-8.58 (d, 1H), 10.89 (5, 1H).MS m/z 540.45 [M-Hr

Statistics shows that 2854-16-2 is playing an increasingly important role. we look forward to future research findings about 1-Amino-2-methylpropan-2-ol.

Reference:
Patent; PFIZER INC.; BAGAL, Sharanjeet Kaur; CUI, Jingrong Jean; GREASLEY, Samantha Elizabeth; LUNNEY, Elizabeth Ann; MCALPINE, Indrawan James; NAGATA, Asako; NINKOVIC, Sacha; OMOTO, Kiyoyuki; SKERRATT, Sarah Elizabeth; STORER, Robert Ian; WARMUS, Joseph Scott; WO2015/170218; (2015); A1;,
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124-68-5, 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. 124-68-5, name is 2-Amino-2-methyl-1-propanol. A new synthetic method of this compound is introduced below.

General procedure: 2-Amino-2-methylpropanol (6, 4.89 g, 55 mmol, 8.5 eq),6.50 mmol of carbonyl compound 4 (1 eq), and 50 mg of H2-activated clay are placed in an autoclave (100 cm3).The sealed reactor is heated for 24 h at various temperatures.After cooling and separation of the H2-clay by filtration,the residue is treated in the same manner asdescribed above. The yields of oxazolidines 7 are given inTable 5.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,124-68-5, 2-Amino-2-methyl-1-propanol, and friends who are interested can also refer to it.

Reference:
Article; Rohand, Taoufik; Savary, Jerome; Marko, Istvan E.; Monatshefte fur Chemie; vol. 149; 8; (2018); p. 1429 – 1436;,
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124-68-5, 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. 124-68-5, name is 2-Amino-2-methyl-1-propanol, 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.

2-amino-2-methyl-1-propanol (4.5g,50.56mmol), sodium bicarbonate (8.4g, 100mmol) and sodium carbonate (10.6g, 100mmol) were mixed in a 250mLreaction flask,, a mixture of dioxane and water (160mL, 3:1) was added, the reaction solution was cooled below 0Cunder an ice bath, a solution of di-tert-butyl dicarbonate (13.1g, 59.82mmol) in dioxane (5mL) was added dropwise under stirring. After completion of the addition, the reaction solution was stirred for 6 hours. After completion of the reaction,dioxane was evaporated under reduced pressure, the residue was extracted with ethyl acetate. The organic phase waswashed with saturated brine, dried over anhydrous sodium sulfate and concentrated. The residue was purified by silicagel column chromatography to give 8.2g product with a yield of 85.77%.

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. 124-68-5, 2-Amino-2-methyl-1-propanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shanghai Pharmaceuticals Holding Co., Ltd.; XIA, Guangxin; LI, Di; ZUO, Hongjian; WU, Guangsheng; DUAN, Lingjun; ZHANG, Jing; MAO, Yu; LIU, Yanjun; (152 pag.)EP3424928; (2019); A1;,
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156-87-6, A common compound: 156-87-6, name is 3-Aminopropan-1-ol,molecular formula is C3H9NO, 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.

To a stirred mixture of 3-aminopropan-1-ol (10.00 mmol, 751 mg) and benzaldehyde (10 mmol, 1061 mg) in dichloromethane (35 ml) was added sodium triacetoxyborohydride (14.00 mmol, 2967 mg). The reaction was stirred overnight then quenched with methanol (200ml) and product isolated by SCX (eluting with 7N ammonia in MeOH). Evaporation gave 0.85 g of 3-(benzylamino)propan-1-ol (51 % yield), EI-MS: m/z = 166.4 [M+H]+.

With the rapid development of chemical substances, we look forward to future research findings about 156-87-6.

Reference:
Patent; N.V. ORGANON; WO2009/37220; (2009); A1;,
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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.110-73-6, name is 2-(Ethylamino)ethanol, molecular formula is C4H11NO, molecular weight is 89.1362, as common compound, the synthetic route is as follows.110-73-6

2-(ethyl(2-hydroxyethyl)amino)benzenesulfonamideTo the solution of 2-fluorobenzenesulfonamide (1051 mg, 6 mmol) in 2-(ethylamino)ethanol (2.93 mL, 30.0 mmol) was heated with microwave irradiation at 130 C for 30 min, heated again with microwave at 130 C for 30 min (71-1), heated again with microwave at 150 C for 30 min. To the reaction mixture was added DMSO (2 mL) and water (0.2 mL) then heated with microwave irradiation at 130 C for 2 h, heated again with microwave at 140 C for 1 h, heated again with microwave at 150 C for 1 h, heated again at 150 C for 5 h. The reaction mixture was diluted with H20 (30 mL), adjusted pH to ~5 with HCI (6 N then 1 N), extracted with EtOAc (3 x 30 mL). The organic layer was washed with brine (30 mL), dried over MgSO4, filtered, concentrated under reduced pressure, purified by silica gel chromatography, to afford the desired product 2-(ethyl(2-hydroxyethyl)amino)benzenesulfonamide (923.0 mg, 3.78 mmol, 63.0 % yield). LC-MS m/z 245 (M + H)+, 0.94 (ret. time).

Statistics shows that 110-73-6 is playing an increasingly important role. we look forward to future research findings about 2-(Ethylamino)ethanol.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; ASTEX THERAPEUTICS LIMITED; BOEHM, Jeffrey Charles; DAVIES, Thomas Glanmor; WOOLFORD, Alison Jo-anne; GRIFFITHS-JONES, Charlotte Mary; WILLEMS, Hendrika Maria Gerarda; NORTON, David; SAXTY, Gordon; HEIGHTMAN, Thomas Daniel; LI, Tindy; KERNS, Jeffrey K.; DAVIS, Roderick S.; YAN, Hongxing; WO2015/92713; (2015); A1;,
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110-73-6, 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. 110-73-6, name is 2-(Ethylamino)ethanol, the common compound, a new synthetic route is introduced below.

Compounds 1 and 2 were prepared by the following procedure: 2-(4-chloro-3-nitrophenyl)-2-oxoethyl 2-aminobenzoate or 2-(4-amino-3-nitrophenyl)-2-oxoethyl 2-aminobenzoate (44.8 mmol) was suspended in polyphosphoric acid (167.3 g). The reaction mixture was heated to 100 C and stirred for 90 min. The mixture was then poured into H2O/crushed ice (700 ml). The precipitated product was filtered, washed with H2O, dried and recrystallized from 2-methoxyethanol. Compounds 3-17 were prepared by the following general procedure: quinolinone 1 (200 mg, 0.63 mmol) was added to a solution of amine (6.3 mmol) and N-methylpyrrolidone (1.0 ml) and the mixture was stirred at 110 C for 2 h. After cooling to room temperature, H2O (20 ml) was added and the pH adjusted to 7 with dilute HCl (1:3). The precipitated solid was collected by suction, washed thoroughly with H2O and dried at 80 C. The crude product was recrystallized from 2-methoxyethanol.

Statistics shows that 110-73-6 is playing an increasingly important role. we look forward to future research findings about 2-(Ethylamino)ethanol.

Reference:
Article; Motyka, Kamil; Hlava?, Jan; Soural, Miroslav; Hradil, Pavel; Krej?i, Petr; Kvapil, Lubomir; Weiss, Milo?; Tetrahedron Letters; vol. 52; 6; (2011); p. 715 – 717;,
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