Tag: M.W=100-200

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. 4720-29-0, name is 3-(Benzylamino)-1-propanol, the common compound, a new synthetic route is introduced below. Computed Properties of C10H15NO

EXAMPLE 20 5-[N-Benzyl-N-(3-hydroxypropyl)amino]-4-chloro-2-methyl-3(2H)-pyridazinone A solution of 11.48 g (64,1 mmol) of 4,5-dichloro-2-methyl-3(2H)-pyridazinone and 31.84 g (193.0 mmol) of 3-(N-benzylamino)propanol in 250 ml of water is boiled for 25 hours while stirring. The mixture is cooled, its pH is set with concentrated hydrochloric acid to 3 and it is extracted with 2*400 ml of ethyl acetate. The organic phase is dried and evaporated, 10 ml of ethyl acetate are added to the evaporation residue, then it is left to stand overnight at -10 C. The precipitated crystals are filtered and washed with ethyl acetate and then with diethyl ether. In this way 10.60 g (54%) of the title compound are obtained with a melting point of 94-95 C.

The synthetic route of 4720-29-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IVAX Drug Research Institute, Ltd.; US6602865; (2003); B1;,
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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.50411-26-2, name is 1-Amino-3-phenylpropan-2-ol, molecular formula is C9H13NO, molecular weight is 151.2056, as common compound, the synthetic route is as follows.HPLC of Formula: C9H13NO

To a solution of E-2-03-2 (the above crude product) in DCM (200 mL) was added (Boc) 20 (18.1 g, 83.3 mmol) dropwise at 0 C. The solution was warmed to r.t. and continued to stir overnight. The solvent was removed under the reduce pressure and the residue was purified by column chromatography on silica gel (ethyl acetate/petroleum ether = 1/100 ~ 1/5) to give E-2-04-2 (3.0 g, 14 % two step) as a yellow oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,50411-26-2, 1-Amino-3-phenylpropan-2-ol, and friends who are interested can also refer to it.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; SAVIRA PHARMACEUTICALS GMBH; EUROPEAN MOLECULAR BIOLOGY LABORATORY; BUSCHMANN, Helmut; SZOLAR, Oliver; HANDLER, Norbert; ROCH, Franz-Ferdinand; CUSACK, Stephen; WEIKERT, Robert; NEIDHART, Werner; SCHULZ-GASCH, Tanja; WOLKERSTORFER, Andrea; (62 pag.)WO2017/46362; (2017); 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. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol. A new synthetic method of this compound is introduced below., name: 4-(Dimethylamino)butan-1-ol

General procedure: 12 (100 mg, 0.35 mmol) was dissolved in the mixture of 1,4-dioxane (10 mL) and H2O (2.00 mL) and then added with boronicacid (2.80 mmol), Pd(dppf)2Cl2 (28 mg, 0.035 mmol) and Cs2CO3(228 mg, 0.70 mmol). The reaction was heated at 100 C underargon atmosphere. After 12 h, the reaction mixture was cooled toroom temperature and was concentrated in vacuo. Then themixture was diluted with water and extracted with ethyl acetate.The combined organic layer was washed by saturated sodiumchloride solution for three times, dried over anhydrous Na2SO4 andconcentrated under reduced pressure. The residue was purified bysilica gel chromatography to give 13.To a stirred solution of 13 and triphosgene (100 mg, 0.34 mmol)in anhydrous dichloromethane (5 mL) was added triethylamine(104 mg, 1.02 mmol) at 0 C under nitrogen atmosphere. After5 min, a solution of 4-(dimethylamino)butan-1-ol (1.02 mmol) indichloromethane (5.00 mL) was added and then the mixture wasstirred at room temperature for overnight. The reactionwas dilutedwith dichloromethane (15 mL) and washed with water (3 20 mL).The organic phases were dried over anhydrous Na2SO4 andconcentrated in vacuo. The residue was purified by using columnchromatography to afford the corresponding product.

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, 13330-96-6, 4-(Dimethylamino)butan-1-ol.

Reference:
Article; Lu, Dong; Liu, Jianan; Zhang, Yunzhe; Liu, Feifei; Zeng, Limin; Peng, Runze; Yang, Li; Ying, Huazhou; Tang, Wei; Chen, Wuhong; Zuo, Jianping; Tong, Xiankun; Liu, Tao; Hu, Youhong; European Journal of Medicinal Chemistry; vol. 145; (2018); p. 328 – 337;,
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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.4728-12-5, name is (2,2-Dimethyl-1,3-dioxan-5-yl)methanol, molecular formula is C7H14O3, molecular weight is 146.18, as common compound, the synthetic route is as follows.Safety of (2,2-Dimethyl-1,3-dioxan-5-yl)methanol

A mixture of 4-chloro-2,3,5-trimethylpyridine 1-oxide (840 g), (2,2-dimethyl-1,3-dioxan-5-yl)methanol (688 g) and toluene (2.52 L) was heated to reflux while removing moisture. While continuing the azeotropic dewatering, the mixture was charged with potassium hydroxide (0.58 kg) over 3 hours and 45 minutes, and the azeotropic dewatering was then continued for another 2.5 hours. The reaction system was cooled to 30°C or less and then charged with ethyl acetate (2.5 L) and 17percent saline solution (3.5 L). The resultant solution was left to stand overnight. The ethyl acetate layer was collected, and the aqueous layer was extracted with ethyl acetate (1.0 L .x. 3). The combined ethyl acetate layers were filtered with Celite and then concentrated under reduced pressure to obtain 1.20 kg of the title compound.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,4728-12-5, (2,2-Dimethyl-1,3-dioxan-5-yl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; Eisai R&D Management Co., Ltd.; EP1875911; (2008); A1;,
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Related Products of 67853-03-6, 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 67853-03-6, name is Methyl 3-(hydroxymethyl)benzoate. This compound has unique chemical properties. The synthetic route is as follows.

General procedure: In a plastic reaction vessel equipped with a Teflon-coated magnetic stiffer was charged DEOXO-FLUOR (6 eq., 2.7 M solution in toluene). To this was then added sequentially 3-acetyl-benzoic acid methyl ester (1 eq.) and ethanol (1 eq.), and the resulting mixture was heated at 85C for 3 days. The reaction mixture was then cooled to RT, diluted with EtOAc and washed with brine. The organic extract was then dried over MgSO4, filtered and the filtrate concentrated in vacuo. Purification of the residue thus obtained by way of column chromatography (Si02, gradient elution, Hex -> 9:1 (v/v) Hex: EtOAc) afforded the intermediate ester as a colorless oil. This was then immediately taken up in methanol (0.1 M), added lithium hydroxide (1 eq.) and then stirred at RT for 16 h. The resulting reaction mixture was carefully neutralized with HC1 (4 M in dioxane) and the volatiles were removed in vacuo. The resulting residue was subjected to column chromatography (Si02, gradient elution, 9:1 (v/v) Hex: EtOAc-> EtOAc) to furnish the desired product as a white solid (68% yield). Prepared in an analogous fashion to Intermediate acid 4, but using 3- hydroxymethyl-benzoic acid methyl ester (1 eq.) in place of 3-acetyl-benzoic acid methyl ester and DAST (1.5 eq.) in place of DEOXO-FLUOR. Furthermore, the reaction took place at -78C over 1 h instead of 85C over 3 days (14% yield).

According to the analysis of related databases, 67853-03-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK PATENT GMBH; JORAND-LEBRUN, Catherine; LAN, Ruoxi; CHEN, Austin; CLARK, Ryan C.; (268 pag.)WO2017/49068; (2017); A1;,
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Synthetic Route of 597-31-9, 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. 597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal, molecular formula is C5H10O2, 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.

Test SetupThe liquid phase hydrogenation was effected over a commercial supported nickel catalyst in the tubular reactor in liquid phase mode. The catalyst volume was 1.8 liters. The hydroxypivalaldehyde-containing crude aldol addition product and hydrogen were supplied continuously at the bottom of the tubular reactor. The hydrogenated material was withdrawn via the top of the tubular reactor, passed into a high-pressure separator and conducted out of the latter by means of level control into an ambient pressure reservoir. The hydrogenation temperature, the hydrogen pressure and the catalyst hourly space velocity were adjusted according to the conditions of the tables which follow. The crude hydroxypivalaldehyde-containing aldol addition product used for the hydrogenation tests had the following typical composition.Organic component (determined by gas chromatography, data in percent): In the analysis data given below for the starting streams, the critical contents for the aliphatic alcohols serving as diluents and the water content were reported. In the analysis of the hydrogenation outputs, the residual contents of HPA and of ester compounds and the NPG content were stated.Liquid phase hydrogenation of HPA at a hydrogenation temperature of 130 C.As a comparison of the test data shows, the proportion of the desired NPG in the hydrogenation output also increases with rising water content in the starting mixture. When, for example, proceeding from test 3, the water content is established below the critical limit of 15% by weight (comparative test 5), the NPG content in the hydrogenation output is lowered. This development is also manifested in tests 6, 7, and 8 (comparative), in which the content of NPG in the hydrogenation output likewise decreases with falling water content in the starting material. The pressure selected in comparative example 9 is no longer sufficient for a satisfactory HPA conversion.

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 597-31-9, 3-Hydroxy-2,2-dimethylpropanal.

Reference:
Patent; Schalapski, Kurt; Kretz, Tonia; Kreickmann, Thosrten; Heymanns, Peter; Lukas, Rainer; Schulz, Rolf-Peter; US2011/98515; (2011); 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. 10488-69-4, name is Ethyl 4-chloro-3-hydroxybutanoate, molecular formula is C6H11ClO3, 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. Quality Control of Ethyl 4-chloro-3-hydroxybutanoate

To 1 L of a 3-necked round bottom flask equipped with a thermometer, a pH meter and a stirrer, 64.8 g of glycinamide hydrochloride, 98.5 g of sodium bicarbonate and 500 mL of ethyl alcohol were successively added and stirred at a room temperature for 1 hour. To the solution, 97.7 g of ethyl- (S)-4-chloro-3-hydroxybutyric was dropwisely added. The reaction solution was further stirred at 80°C for 20 hours. Work-up procedures were performed in the same manner as mentioned in the Example 7. Recrystallization with methyl alcohol and acetone gave 52.5 g of the targeted (S)-4-hydroxy-2-oxo- I -pyrrolidine acetamide.

With the rapid development of chemical substances, we look forward to future research findings about 10488-69-4.

Reference:
Patent; AHN-GOOK PHARMACEUTICAL CO., LTD.; RSTECH CORPORATION; WO2005/115978; (2005); A1;,
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Adding a certain compound to certain chemical reactions, such as: 767-90-8, (2-Ethylphenyl)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, 767-90-8, blongs to alcohols-buliding-blocks compound. Recommanded Product: 767-90-8

Step 1: A solution of (2-ethylphenyl)methanol (500 mg, 3.67 mmol) and triethylamine (742 mg, 7.34 mmol) in DCM (5 mL) was added MsCI (1.0 g, 8.73 mmol) at 000 and stirred at 000 for 0.5 hour. Then it was stirred at 20C for 1 hour. The mixture was quenched with water (0.5 mL), and diluted with DCM (10 mL). The mixture was added NaHCO3 (aq.) until pH=8. The organic layer was washed with water (3 x 5 mL), dried with an hydrous Na2504, filteredand concentrated under vacuum to give 2-ethylbenzyl methanesulfonate (600 mg), which was used into the next step without further purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,767-90-8, its application will become more common.

Reference:
Patent; H. LUNDBECK A/S; KEHLER, Jan; RASMUSSEN, Lars, Kyhn; LANGGARD, Morten; JESSING, Mikkel; VITAL, Paulo, Jorge, Vieira; JUHL, Karsten; (159 pag.)WO2016/174188; (2016); A1;,
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Reference of 623-50-7 ,Some common heterocyclic compound, 623-50-7, molecular formula is C4H8O3, 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.

1 (100.0 g, 960.52 mmol) and imidazole (77.3 g, 1.15 mol)Soluble in dichloromethane (1.5L),Under an ice bath, tert-butyldiphenylchlorosilane (264.0 g, 960.52 mmol) was slowly added dropwise using a constant pressure dropping funnel.After the addition is completed,Transfer to room temperature for 16 h.filter,The filtrate was washed with a 1.0 mol/L hydrochloric acid solution (300 ml × 2).The dichloromethane layer was washed with a saturated sodium bicarbonate solution (100 ml x 2).Dry over anhydrous sodium sulfate,Concentrated to a white clear liquid 2 (297.7 g, 91%).

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. 623-50-7, Ethyl 2-hydroxyacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Guangzhou Yue Mei Pharmaceutical Technology Co., Ltd.; Guo Zhongwu; Hao Linghua; Zhong Bohua; Zheng Junxia; (10 pag.)CN108997429; (2018); A;,
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Reference of 10488-69-4, Adding some certain compound to certain chemical reactions, such as: 10488-69-4, name is Ethyl 4-chloro-3-hydroxybutanoate,molecular formula is C6H11ClO3, 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 10488-69-4.

Example 1 Preparation of (S)-Ethyl-3-hydroxy-4-(1-phenyl-1H-tetrazol-5-ylthio)butanoate (11a) 121.2 g of triethylamine and 100 g of (S)-4-chloro-3-hydroxybutyric acid ester were added to the solution of 96.2 g of 1-phenyl-1H-terazole-5-thiol in 750 mL toluene at 25° C. The reaction mixture was heated to 80° C. to 85° C. for completion of reaction on TLC. The reaction mixture was cooled to 25° C. and treated with 200 mL of water and stirred to separate the layers. The separated aqueous layer was twice extracted with 100 mL toluene. The combined organic layer was treated with 300 mL HCl solution followed by washing with 200 ml water. The organic layer was distilled under vacuum below 50° C. The residue was treated with 200 ml hexane and stirred for 30 minutes. The solution was distilled under vacuum below 50° C. to remove hexane and obtain (S)-Ethyl-3-hydroxy-4-(1-phenyl-1H-tetrazol-5-ylthio)butanoate (11a) as an oil.

According to the analysis of related databases, 10488-69-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Dwivedi, Shriprakash Dhar; Patel, Dhimant Jasubhai; Rupapara, Mahesh Laljibhai; US2013/158263; (2013); A1;,
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