Category: 100-37-8

Electric Literature of 100-37-8 , The common heterocyclic compound, 100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, 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.

260 g of thionyl chloride and 240 g of dichloromethane were added to a 1 L reaction flask to cool down, and a mixed solution of 120 g of diethylaminoethanol and 100 g of dichloromethane was prepared in a 500 ml beaker during the cooling process, when the temperature in the reaction flask was lowered to – 10 C,While maintaining the temperature in the range of -10 C to 20 C, a mixture of diethylaminoethanol and dichloromethane was added dropwise, and after the completion of the dropwise addition, the temperature was raised to 35 C for 2.5 h, and then the dichloromethane was concentrated and concentrated until not. After concentration, the temperature was lowered to 24 C. 220 g of anhydrous methanol was added to the reaction flask and heated to dissolve the solid. After the solid was completely dissolved, the ice brine was cooled to -8 C for 7 h.Filtering to obtain 2-diethylaminochloroethane hydrochloride wet product,After the mother liquor is collected, the methanol is continuously concentrated and recovered, and the residue is subjected to freeze crystallization for 24 hours.The mother liquor product is obtained by suction filtration, and the mother liquor product is recrystallized with methanol.The obtained 2-diethylaminochloroethane hydrochloride is dried at 55-60 C to obtain a dry product.The purity of the liquid phase was determined to be 99.74%, and the molar yield was 98.08%.

The synthetic route of 100-37-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Baoji University of Arts and Sciences; Guo Yaning; (6 pag.)CN108863811; (2018); A;,
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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.100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, molecular weight is 117.1894, as common compound, the synthetic route is as follows.HPLC of Formula: C6H15NO

A mixture of 3-[6-(7-chloro-4-oxo-4H-1,3-benzothiazin-2-yl)-4-(methylsulfonyl)pyridin-2-yl]prop anoic acid (0.21 g, 0.5 mmol), N,N-diethylethanolamine (0.12 g, 1.0 mmol), HOBt H2O (92 mg, 0.6 mmol), WSC (116 mg, 0.6 mmol), 4-dimethylaminopyridine (74 mg, 0.6 mmol) and DMF (3 ml) was stirred at room temperature for 18 hours. Water (20 ml) was added to the reaction mixture and the crystals formed were taken by filtration. The crystals were recrystallized from ethanol to give the title compound (0.13 g, 50%). Melting point: 150.5-151.5C 1H-NMR (CDCl3) delta: 1.02 (6H, t, J=7.2 Hz), 2.57 (4H, q, J=7.2 Hz), 2.71 (2H, t, J=6.3 Hz), 3.04 (2H, t, J=7.2 Hz), 3.16 (3H, s), 3.39 (2H, t, J=7.2 Hz), 4.20 (2H, t, J=6.3 Hz), 7.60-7.67 (2H, m), 7.98 (1H, s), 8.50 (1H, d, J=8.4 Hz), 8.80 (1H, s).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,100-37-8, 2-(Diethylamino)ethanol, and friends who are interested can also refer to it.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP1897880; (2008); A1;,
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Synthetic Route of 100-37-8 , The common heterocyclic compound, 100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, 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.

alpha-methyl-4-(2-thienylcarbonyl)benzene acetyl chloride 28.1g (0.1mol) was dissolved in chloroform 100ml . The mixture was cooled to 0. Triethylamine 15ml and diethylaminoethanol 11.7g (0.1mol) were added to the reaction mixture. The mixture was stirred for 3 hours at room temperature. The solvent was evaporated. The residue was dissolved in methanol (300ml), and 5% sodium bicarbonate (200ml) was added to the reaction mixture. The mixture was stirred for 3 hours. The mixture was evaporated and dried. methanol (300 ml) was added to the residue with stirring. The solid was removed by filtration, and washed with methanol. The solution was evaporated to dryness, and the residue was dissolved in chloroform (200ml). acetic acid 6g was added to the reaction mixture with stirring. Some of the solid matters were removed by filtration. another acetic acid 6g was added to the reaction mixture while Stirring. The organic solution was evaporated. After drying, the desired product 35g (83.2%) was obtained.

The synthetic route of 100-37-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Techfields Biochem Company Limited; Yu, Chauncy; Shu, Rina; (52 pag.)JP2016/130241; (2016); A;,
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100-37-8 , The common heterocyclic compound, 100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, 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) Synthesis: 240 g (2.4 mol) of methyl methacrylate,117 g (1.0 mol) of diethylaminoethanol, 200 g of n-hexane,8 g of lithium hydroxide and 0.5 g of phenothiazine were added with stirring,Thermometer and water separator in a 1000 mL three-necked flask,Heated to 65 C ~ 73 C, constantly reflux and separation of methanol,The reaction was stopped (about 5 h) after refluxing to the absence of methanol separation.34.5 g of methanol was separated,Gas chromatographic analysis showed that the methanol content was 88.6%The methyl methacrylate content was 11.2%.(2) purification: cooling to room temperature, add 300mL ¡Á 2 of deionized water washed twice. The oil was gradually decompressed (0 to 100 mmHg) at 60 C to 100 C,Unreacted methyl methacrylate and diethylaminoethanol,And then diethyl etherate methacrylate was distilled off under reduced pressure at 5 to 10 mmHg and 90C to 100C. The resulting product was 175.7 g (theoretical yield 185.26 g) in a yield of 94.1%.Gas chromatographic analysis showed that the content of diethylaminoethyl methacrylate was99.2%.

According to the analysis of related databases, 100-37-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Qingdao University of Science and Technology; Tang Linsheng; Yang Jingwei; Wu Hongzhi; Hou Xiaomin; Zhu Xin; Mi Chengjing; (9 pag.)CN106966913; (2017); A;,
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Adding a certain compound to certain chemical reactions, such as: 100-37-8, 2-(Diethylamino)ethanol, 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, 100-37-8, blongs to alcohols-buliding-blocks compound. 100-37-8

0 C, under Ar protection,To NaH (60%, 1.1g, 27.01mmol, 2.5eq)Compound 2 (1.52 g, 12.97 mmol, 1.2 eq) was added dropwise to a solution of THF (15 mL)Of THF (5 mL).Stir at 0 C for 15 min.Compound 1 (2.0 g, 10.80 mmol, 1.0 eq) was added.Stir overnight at room temperature. The reaction was quenched with saturated NH4Cl.The reaction solution was concentrated under reduced pressure, diluted with water (40 mL), washed with PE: EtOAc = 10: 1 (40 mL), and adjusted to pH = 4 with 5M aq.Filtration gave compound 3 (3.0 g, 82%) as a white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,100-37-8, its application will become more common.

Reference:
Patent; Longtaishen Pharmaceutical (Nanjing) Co., Ltd.; Yang Lei; (55 pag.)CN110698460; (2020); A;,
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100-37-8, 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. 100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, 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: Under air atmosphere, a reaction tube was charged with disulfide (0.2 mmol), Tertiary amine (0.4 mmol), I2 (0.4 mmol) Na2CO3 (0.4 mmol) and DMSO (2 mL). The vessel was sealed and heated at 100 C (oil bath temperature) for 24 h and then cooled to room temperature. The reaction mixture was washed with saturated Na2S2O3(2 x 15 mL) and then brine (1 x 15 mL). After the aqueous layer was extracted with ethyl acetate, the combined organic layers were dried over anhydrous Na2SO4 and evaporated under vacuum. The residue was purified by flash column chromatography (hexane/ethyl acetate) to afford the desired products.

The chemical industry reduces the impact on the environment during synthesis 100-37-8, I believe this compound will play a more active role in future production and life.

Reference:
Letter; Gao, Xu-Hong; Xu, Wei; Zhang, Xing-Guo; Deng, Chen-Liang; Synlett; vol. 28; 7; (2017); p. 841 – 846;,
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100-37-8, 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. 100-37-8, name is 2-(Diethylamino)ethanol, molecular formula is C6H15NO, 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.

Example 32; N-cyclopropyl-3-({4-[(6-{ [2-(diethylamino) ethoxy] methyl} pyridin-2- yl) methoxy] benzoyl} amino)-4-methylbenzamide To a 60% dispersion of NaH in mineral oil (25 mg, 0.625 mmol) in DMA (4 mL) was added N,N-diethylethanolamine (24 mg, 0.205 mmol). The reaction was stirred at room temperature for 20 minutes. A solution of 3- [ (4- { [6- (bromomethyl) pyridin-2- yl] methoxy benzoyl) amino]-N-cyclopropyl-4-methylbenzamide (77 mg, 0.155 mmol) in DMA (2 mL) was added dropwise to the reaction which was then stirred for 1 h at room temperature. The reaction was quenched by the addition of water (1 mL) and was purified by preparative HPLC to give the title compound as a white solid (29 mg, 35%); NMR Spectrum: (DMSOd6) 0.58 (m, 2H), 0.69 (m, 2H), 0.96 (t, 6H), 2.26 (s, 3H), 2.50 (m, 4H), 2.64 (t, 2H), 2.86 (m, 1H), 3.59 (t, 2H), 4.59 (s, 2H), 5.75 (s, 2H), 7.18 (d, 2H), 7.33 (d, 1H), 7.42 (m, 2H), 7.64 (dd, 1H), 7.80 (s, 1H), 7. 87 (t, 1H), 7.96 (d, 2H), 8. 36 (d, 1H), 9.83 (s, 1H) ; Mass Spectrum : M+H+ 531.

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. 100-37-8, 2-(Diethylamino)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2005/61465; (2005); A1;,
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100-37-8, 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. 100-37-8, name is 2-(Diethylamino)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

j0044] Example 2: a bis (2-diethylaminoethyl) ether synthesizing method using N,N-diethylethanolamine, diethylamine and ethyne as raw materials (original raw materials) is performed by the following steps in proper order:10045] step 1: synthesizing:10046] wherein at a room temperature, 117 g N,N-diethylethanolamine (1.0 mol), 268 g diisobutyl ether (as a solvent) and 3.6 g sodium ethoxide are added in a high-pressure reaction dave with a mixing and temperature-measuring device; the dave cover is put on and leakage is inspected; then 6.5 g ethyne (0.25 mol) and 55.0 g diethylamine (0.75 mol) are forced into the dave in proper order; afier feeding, a temperature is raised to 50 C., and kept on for 7 h before completing the reaction;10047] afier reaction, the dave is opened and a filtrate is obtained by filtering the reaction mixture; and step 2:10048] distilling the filtrate obtained at 60 C. and atmospheric pressure for half an hour for the unreacted diethylamine to come out; then proceeding to rectification at reduced pressure intermittently; at a pressure of 1 kPa, collecting the previous fractions (all fractions before 91 C.)- unreacted N,N-diethylethanolamine and solvent; then collecting the fractions at 9 1-93 C. and obtaining bis (2-diethylaminoethyl) etherweighing 51.5 g; wherein a product purity is 99.1%; by taking the consumed ethyne as reference, a yield rate is 95.3%.

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 100-37-8, 2-(Diethylamino)ethanol.

Reference:
Patent; SICHUAN ZHIJIANG ADVANCED MATERIALS CO., LTD.; Zhang, Chao; Zhang, Hua; Ye, Xiaoming; Zhang, Qi; Ye, Chuanwei; US2015/291506; (2015); A1;,
Alcohol – Wikipedia,
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Some common heterocyclic compound, 100-37-8, molecular formula is C6H15NO, 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.100-37-8

To a 250 ml four-necked flask equipped with a stirrer and a water separator and a reflux device was added 16.6 g (0.1 mol) of phthalic acid,35.1 g (0.3 mol) of N, N-diethylaminoethanol,0.8 g of titanium sulphate, 20 ml of xylene,Stirring heated to 150 reflux reaction 5h,Until 3.6 g (0.2 mol) of water was separated,The catalyst was removed by filtration (direct reuse)The filtrate was transferred to another 250 ml three-necked flask,The solvent was distilled off under reduced pressure (recovered)Excessed diethylaminoethanol (recycled) and low boiling materials,Add 3.0 g of activated clay to stir for 30 minutes,Cooling to 80 below,Filter yellowColor oil-like liquid phthalic acid bis-diethylaminoethanol ester 35.67g,Yield 90.8%.againThe bis-diethylaminoethacrylate phthalate was mixed with twice as much as citric acid and heated to 120 C,After the citric acid melts,Stirring down the crystallization of salt,To obtain a white powdery solid product, bis-diethylaminoethanol citrate citrate.

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 100-37-8.

Reference:
Patent; Suzhou University of Science and Technology; Wang, Yanlin; Wang, Hao; Wang, Yan; Shao, Wei; (13 pag.)CN106008238; (2016); A;,
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100-37-8, 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. 100-37-8, name is 2-(Diethylamino)ethanol. A new synthetic method of this compound is introduced below.

25 g of 4-cyano-4-(thiobenzylthio) pentanoic acid (89.6 mmol) were dissolved in 100 g of tetrahydrofurane anhydride. Under a nitrogen atmosphere, 15.726 g of 10-hydroxy benzotriazole (0.116 mol) were added thereto and stirred for 30 minutes. 22.72 g ethyldimethylaminocarboimide (0.116 mol) were added and stirred for 15 minutes, followed by the addition of 11.98 g of dimethylaminoethanol (0.134 mol) and stirring at room temperature for 6 hours. After completing the reaction, the resultant was extracted with water and diethyl ether and dried over magnesium sulfate. The organic solvent was vacuum distillated. It was purified with a column to obtain 21.95 g of 4-cyano-4-(thiobenzylthio)pentanoic dimethylamino ethyl ester (70% yield). 16.9 g of the obtained 4-cyano-4-(thiobenzylthio) pentanoic acid (48.4 mmol) were dissolved in 100 g of tetrahydrofurane anhydride. Under a nitrogen atmosphere, 8.496 g of 10-hydroxy benzotriazole (0.0629 mol) were added thereto, and stirred for 30 minutes. 12.26 g of ethyldimethylaminocarboimide (0.0629 mol) were added and stirred for 15 minutes, followed by addition of 11.47 g of diethylaminoethanol (0.0981 mol). The stirring was continued at room temperature for 12 hours. After completing the reaction, the resultant was extracted with water and diethyl ether, and dried over magnesium sulfate. The organic solvent was distillated in a vacuum, then purified with a column to obtain 12.8 g of 4-cyano-4-(thiobenzylthio)pentanoic diethylamino ethyl ester (70% yield). 12.7 g of the obtained 4-cyano-4-(thiobenzylthio) pentanoic acid (36.39 mmol) were dissolved in 60 g tetrahydrofurane anhydride. Under a nitrogen atmosphere, 6.36 g of 10-hydroxy benzotriazole (0.0473 mol) were added thereto and stirred for 30 minutes. 9.22 g of ethyldimethylaminocarboimide (0.0473 mol) were added and stirred for. 15 minutes, followed by the addition of 7.9 g of diisopropylene diamine (0.0546213 mol) and stirring at room temperature for an additional 12 hours. After completing the reaction, the resultant was extracted with water and diethyl ether, and dried over magnesium sulfate. The organic solvent was distillated under vacuum, and purified with a column to obtain 10.35 g of 4-cyano-4-(thiobenzylthio)pentanoic diisopropyl amino ethyl ester (70% yield).

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. 100-37-8, 2-(Diethylamino)ethanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Kim, Hee-Jung; Kim, Dong-Ryul; US2004/138492; (2004); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts