Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 311-86-4, 2-Bromo-3,3,3-trifluoropropan-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, Quality Control of 2-Bromo-3,3,3-trifluoropropan-1-ol, blongs to alcohols-buliding-blocks compound. Quality Control of 2-Bromo-3,3,3-trifluoropropan-1-ol

54 g of 2-bromo-3,3,3-trifluoropropanol, 79 g of methanol, 9.7 g of activated RaneyNi catalyst and 19.3 g of potassium carbonate were charged into a 300 mL autoclave, stirred, evacuated and replaced with hydrogen After three times, pressure 5Mpa, heated to 80 C, the reaction 3.0h, stop the reaction, cooling, discharge, distillation to 3,3,3 – trifluoropropanol; Yield 95.0%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,311-86-4, 2-Bromo-3,3,3-trifluoropropan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; Xi’an Modern Chemistry Research Institute; Gu, Yujie; Lu, Jian; Ma, Hui; Wang, Zhixuan; Kang, Jianping; Du, Yongmei; Tu, Donghuai; Wan, Hong; Li, Yang; (5 pag.)CN105399607; (2016); A;,
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Electric Literature of 57772-50-6 ,Some common heterocyclic compound, 57772-50-6, molecular formula is C8H11NO, 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.

General procedure: To an oven-dried 15 mL sealed tube were added 2-aminophenylmethanol 1 (0.425 mmol), benzonitrile 2(0.25 mmol), Ru cat. b (1.94 mg, 1 mol%), and KOtBu (14.02 mg, 0.5equiv) intamyl alcohol (1 mL) under an air atmosphere. The sealedtube was capped and heated at 130C for 2 h. The reaction mixturewas cooled down to room temperature and directly concentratedunder vacuum. The crude mixture was puried by preparative thin-layer-chromatography (petroleum ether/ethyl acetate 20/1) togive the desired product 3 or 4.

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. 57772-50-6, (2-Amino-3-methylphenyl)methanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Wan, Xiao-Min; Liu, Zi-Lin; Liu, Wan-Qing; Cao, Xiao-Niu; Zhu, Xinju; Zhao, Xue-Mei; Song, Bing; Hao, Xin-Qi; Liu, Guoji; Tetrahedron; vol. 75; 18; (2019); p. 2697 – 2705;,
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Reference of 86770-74-3 ,Some common heterocyclic compound, 86770-74-3, molecular formula is C8H19NO4, 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.

An oven-dried 200 mL round bottomed flask was charged with Biotin-NHS (1.17 g, 3.43 mmol) and 2-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)ethan-1-ol (730 mg, 3.80 mmol). The flask was subjected to three cycles of vacuum/nitrogen backfill before addition of anhydrous DMF (69 mL). To the colorless solution was added triethylamine (960 muL, 6.85 mmol) and after 45 minutes, the solution was concentrated in vacuo. The crude material was purified by flash chromatography (basic alumina: 5 % methanol in CH2Cl2) to provide the title compound as an opaque amorphous solid (1.18 g, 2.81 mmol, 82 % yield). 1H NMR (400 MHz, CDCl3) delta: 7.21 (1H, br t), 5.97 (1H, br s), 5.09 (1H, br s), 4.48 (1H, m), 4.30 (1H, m), 3.78 (1H, m), 3.70 (4H, m), 3.65-3.58 (8H, m), 3.52 (2H, m), 3.41 (2H, m), 3.13 (1H, td, J = 7.4, 4.6 Hz), 2.90 (1H, dd, J = 12.8, 5.0 Hz), 2.73 (1H, d, J = 12.8 Hz), 2.20 (2H, t, J = 7.5 Hz), 1.78 (4H, m), 1.46-1.38 (2H, m); 13C NMR (100 MHz, CDCl3) delta: 173.49, 164.17, 72.60, 70.51, 70.32, 70.17, 70.00, 69.92, 61.78, 61.41, 60.22, 55.65, 40.47, 39.08, 35.90, 28.30, 28.11, 25.69. IR numax/cm-1 (film): 3273, 3085, 2916, 2865, 1690, 1669, 1646, 1551, 1464, 1420, 1264, 1240, 1202, 1101, 869, 693. m/z HRMS (ESI): [M+ H]+ calculated for C18H33N3O6S+ = 442.1982, found 442.1962.

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. 86770-74-3, 2-(2-(2-(2-Aminoethoxy)ethoxy)ethoxy)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Nottingham, Kyle G.; McNally, Andrew; McNaughton, Brian R.; Tetrahedron Letters; vol. 59; 3; (2018); p. 234 – 237;,
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Related Products of 4152-92-5 , The common heterocyclic compound, 4152-92-5, name is (2-(Aminomethyl)phenyl)methanol, molecular formula is C8H11NO, 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.

An ice-cold pyridine solution (10 mL) of compound 23 (1 mmol) is treated successively, in a dropwise fashion with acetyl chloride (1 mmol), then after 5 min with MsCl (1.1 mmol). The solution is warmed to room temperature then the solvent is removed. The residue is dissolved in EtOAc, washed with water, dried (MgS04), filtered and concentrated in vacuo. Purification by column chromatography affords pure compound 24.

The synthetic route of 4152-92-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ONTORII, INC.; BUTLER, David; IWAMOTO, Naoki; MEENA, Meena; SVRZIKAPA, Nenad; VERDINE, Gregory L.; ZLATEV, Ivan; WO2014/12081; (2014); A2;,
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Related Products of 115-20-8 ,Some common heterocyclic compound, 115-20-8, molecular formula is C2H3Cl3O, 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 stirring solution of 5-chloro-2-(quinolin-6-yl)benzoic acid (0.201 g, 0.708 mmol) and TEA (0.148 ml, 1.06 mmol) in 1 ,4-dioxane (10 ml) at RT, was added DPPA (0.191 ml, 0.244 mmol). After stirring for 30 min at RT, 2,2,2-trichloroethanol (0.680 ml, 7.08 mmol) was added and the reaction was stirred with heating at 100 C for 2 h. The completed reaction was diluted with brine (10 ml) and extracted with EtOAc (3×25 ml). The combined organics were washed with 5% citric acid (10 ml), sat’d. NaHC03 (10 ml) and brine (10 ml), dried (MgSO^, concentrated in vacuo and purified by chromatography to afford 2,2,2-trichloroethyl 5-chloro-2-(quinolin-6- yl)phenylcarbamate (0.25 g, 82% yield) as a white solid. MS (ESI) m/z: 431.0 (M+H+).

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; DECIPHERA PHARMACEUTICALS, LLC; FLYNN, Daniel L.; PETILLO, Peter A.; KAUFMAN, Michael D.; WO2013/36232; (2013); A2;,
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Related Products of 60211-57-6, 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. 60211-57-6, name is 3,5-Dichlorobenzyl alcohol. A new synthetic method of this compound is introduced below.

To a solution of 3.5 g of 3,5-dichlorobenzyl alcohol (Aldrich) in 75 mL of dichloromethane at 0C was added 1.8 mL of methane sulfonylchloride followed by 3.5 mL of triethylamine added dropwise. After 2 hours the solution was diluted to 150 mL with dichloromethane, washed with 3N HCl, saturated aqueous NaHCO3 dried with Na2SO4 and the solvents removed to yield the desired 3,5-dichlorobenzyl methanesulfonate as a yellow oil that was used without purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,60211-57-6, 3,5-Dichlorobenzyl alcohol, and friends who are interested can also refer to it.

Reference:
Patent; ELAN PHARMACEUTICALS, INC.; ELI LILLY AND COMPANY; EP951466; (2009); B1;,
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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. 4461-39-6, name is N-(2-Hydroxyethyl)-1,3-propanediamine. A new synthetic method of this compound is introduced below., category: alcohols-buliding-blocks

To a round-bottom flask (250 mL) containing 3-(benzyloxy)benzaldehyde (3.50 g, 16.5 mmol) dissolved in methanol (100 ml), N-(2-Hydroxyethyl)-1,3-propanediamine (3.50 g, 16.5 mmol) was added. The resulting mixture was stirred for 2 h at ambient temperature. Then carbon disulfide (1.00 mL, 16.5 mmol) was slowly mixed to the reaction, which was kept under stirring for about 40 min. Cu(O2CCH3)2H2O (1.50 g, 8.25 mmol) was then added and a brown solid was formed. After stirring for 4 h, the formed brown precipitate was filtrated and re-crystallized in a 4:1 mixture of CH2Cl2 and toluene. Yield 81%. Mp. 93.6-95.0 C. IR (cm-1, KBr): 1496 (nuN-CS); 980 {nuasym(C-S)}; 601 {nusym(C-S)}. Analysis of C, H and N, respectively for C40H48N4O4S4Cu found% (calc.%): 56.95 (57.15); 5.67 (5.76); 6.58 (6.66).

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, 4461-39-6, N-(2-Hydroxyethyl)-1,3-propanediamine.

Reference:
Article; Ferreira, Isabella P.; Lima, Geraldo M. De; Paniago, Eucler B.; Takahashi, Jacqueline A.; Krambrock, Klaus; Pinheiro, Carlos B.; Wardell, James L.; Visentin, Lorenzo C.; Journal of Molecular Structure; vol. 1048; (2013); p. 357 – 366;,
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Reference of 3250-73-5 , The common heterocyclic compound, 3250-73-5, name is 2-(2-Ethoxyphenoxy)ethanol, molecular formula is C10H14O3, 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.

Afterthe pyridine (200ml) was added to obtained 2 – (2- ethoxyphenoxy) ethanols (50.0g,0.274mol, 1.0eq) at 1 step and it altogether dissolved it cooled at 0. Methanesulfonyl chlorides(35.0ml, 0.453mol, 1.65eq) were dipped from the gradually to the cooledsolution and it was stirred for 1 hour while it heated to the slowly to the room temperature (20). The solid which wasgenerated after it dipped the water (350ml) as the gradually after it cooledthe above-mentioned stirred solution at 0 was filtered and 2 – (2- ethoxyphenoxy) ethylmethane sulfonate was obtained (62g, and the yield 87%). 2-(2-) NMR . Theobtained NMR peak of 2 – (2- ethoxyphenoxy) ethyl methane sulfonate showed uplike the next.

The synthetic route of 3250-73-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Boryung Pharmaceutical Co., Ltd; Kim, Ji Han; Myung, Jae Hyok; Lee, Jun Kwang; Sun, Yong Ho; Kim, Hak Do; (20 pag.)KR101525493; (2015); B1;,
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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 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of 3-Hydroxy-2,2-dimethylpropanal

EXAMPLE 2Purification of HPA A complete mixture was prepared at 55C by adding 2505 parts of water into 835 parts of the crude HPA obtained in Reference Example 1. The mixture was gradually cooled from 55C to 32C over 5 h under stirring and then kept at 32C for one hour. The resultant crystals were separated by solid-liquid separation using a top-discharge centrifugal separator and then washed with water, to obtain HPA having a purity of 96.5% by weight in 60% recovery. The water content was 12% by weight and the remaining TEA content was 0.01% by weight. Synthesis of SPG from Purified HPA Into a solution of 95 parts of PE in 1200 parts of water, were added 5 parts of p-toluenesulfonic acid (PTSA) and 26 parts of SPG crystals obtained in Reference Example 2 as seed crystals (1.7% by weight of the total feed amount into the reaction system). Then, an aqueous solution of the purified HPA prepared by dissolving 160 parts of the purified HPA in 65 parts of water under heating at 80C was further added dropwise over 3.5 h. The SPG content X was 14.8% by weight. The pH of the reaction liquid at the initiation of reaction was 1.8, and the reaction temperature was 90C. After the dropwise addition, the reaction liquid was aged for 2 h while maintaining the temperature at 90C. The pH of the reaction production solution at the completion of reaction was 1.8. After the aging, the reaction product solution was separated into wet SPG and 1240 parts of reaction mother liquor by solid-liquid separation. The wet SPG was washed with 460 parts of water and then dried, to obtain 147 parts of SPG crystals. The yield of SPG was 56.8 mol% based on the charged PE, and the purity of SPG crystals was 99.9% by weight when analyzed by GC. The average particle size of SPG crystals was 23 um when measured on a water dispersion of SPG crystals by using a wet particle size distribution analyzer after exposing the water dispersion to ultrasonic wave for 10 min. The amount of waste water (reaction mother liquor + recovered washings + recovered water in drying) was 1780 parts. During the solid-liquid separation by filtration through a glass filter under reduced pressure, no crack occurred on the cake. The liquid content of SPG cake immediately after the filtration was 37% by weight. First Recycling Reaction Next, a first recycling reaction was performed in the same manner as in the above synthesis except for making 1200 parts of the reaction mother liquor (85% by weight of the whole amount) and 95 parts of PE into a solution under heating and using 0.7 part of PTSA and 240 parts of the aqueous solution of the purified HPA. The yield of dried SPG was 96.5 mol% and the purity was 99.8% by weight. The average particle size after exposed to ultrasonic wave was 22 um. During the solid-liquid separation by filtration through a glass filter under reduced pressure, no crack occurred on the cake. The liquid content of SPG cake immediately after the filtration was 37% by weight. Second Recycling Reaction Next, a second recycling reaction was performed in the same manner as in the first recycling reaction except for using 1100 parts of the reaction mother liquor (83% by weight of the whole amount) and 100 parts of water. The yield of dried SPG was 94.6 mol% and the purity was 99.8% by weight. The average particle size after exposed to ultrasonic wave was 22 um. During the solid-liquid separation by filtration through a glass filter under reduced pressure, no crack occurred on the cake. The liquid content of SPG cake immediately after the filtration was 37% by weight. Third and Subsequent Recycling Reactions The above procedure was repeated to perform the recycling reactions up to 10 cycles. The yield of SPG was 94.0 mol%, the purity was 99.7% by weight, and the particle size after exposed to ultrasonic wave was 20 um or more, each in average of third to tenth recycling reactions. The amount of waste water was 584 parts in average. During the solid-liquid separation by filtration through a glass filter under reduced pressure, no crack occurred on the cake. The liquid content of SPG cake immediately after the filtration was 42% by weight in average.

With the rapid development of chemical substances, we look forward to future research findings about 597-31-9.

Reference:
Patent; MITSUBISHI GAS CHEMICAL COMPANY, INC.; EP1598357; (2005); A1;,
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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. 22348-44-3, name is trans-4-(Methylamino)cyclohexanol. A new synthetic method of this compound is introduced below., COA of Formula: C7H15NO

To a solution of compound 84-2 (140 mg, 1.085 mmol) in DCM (4 mL) was added Boc anhydride (473 mg, 2.170 mmol) and TEA (329 mg, 3.255 mmol), and the reaction solution was stirred at 20 C. for 30 min. After of TLC indicated the reaction was complete, the reaction was quenched with water (30 mL¡Á1), and the aqueous phase was extracted with EtOAc (50 mL¡Á2). Then the organic phases were combined, dried over anhydrous Na2SO4, filtered and evaporated to give compound 84-3 (yellow oil, 180 mg, Yield 72.4%). 1H NMR (400 MHz, CDCl3): delta ppm 6.31 (br. s., 1H), 5.14-5.21 (m, 1H), 4.97 (d, J=6.24 Hz, 2H), 4.48 (d, J=7.09 Hz, 2H), 3.36 (t, J=11.49 Hz, 1H), 2.85 (t, J=11.62 Hz, 1H), 2.18 (br. s., 1H), 1.89 (br. s., 1H), 1.60-1.66 (m, 1H), 1.47 (t, 3H), 1.44 (s, 9H). (1362) LCMS (ESI) m/z: 230 (M+1)

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, 22348-44-3, trans-4-(Methylamino)cyclohexanol.

Reference:
Patent; Hubei Bio-Pharmaceutical Industrial Technological Institute Inc.; Humanwell Healthcare (Group) Co., Ltd.; Wang, Xuehai; Wu, Chengde; Xu, Yong; Shen, Chunli; Li, Li’e; Hu, Guoping; Yue, Yang; Li, Jian; Guo, Diliang; Shi, Nengyang; Huang, Lu; Chen, Shuhui; Tu, Ronghua; Yang, Zhongwen; Zhang, Xuwen; Xiao, Qiang; Tian, Hua; Yu, Yanping; Chen, Hailiang; Sun, Wenjie; He, Zhenyu; Shen, Jie; Yang, Jing; Tang, Jing; Zhou, Wen; Yu, Jing; Zhang, Yi; Liu, Quan; (251 pag.)US2017/313683; (2017); A1;,
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