Category: 645-36-3

Electric Literature of 645-36-3,Some common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, molecular formula is C6H15NO2, 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: The reaction mixture containing 0.5 g (1.8 mmol) of 4-(dibromomethyl)benzenecarbaldehyde (7), 0.11 g (0.0018 mmol) of isopropylamine (12) and 0.2 g of molecular sieves 3 A in 10 mL of dry benzene was thermostated at room temperature for 24 h. N-Isopropyl-4-(dibromomethyl)benzenecarbimine (14) (0.44 g, 77%) in the form of yellow oil was obtained by filtration through the molecular sieves followed by the removal of the solvent in vacuo provided by water jetpump.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,2-Diethoxyethanamine, its application will become more common.

Reference:
Article; Gazizov; Ivanova, S. Yu.; Karimova; Bagauva; Gazizova; Karimova; Russian Chemical Bulletin; vol. 65; 1; (2016); p. 191 – 194; Izv. Akad. Nauk, Ser. Khim.; 1; (2016); p. 191 – 194,4;,
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Application of 645-36-3, These common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, 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.

2,2-Diethoxyethylamine (430 muL, 2.95 mmol) and Na2CO3 (0.285g, 2.69 mmol) were added to a stirred soln of pyrimidine 717 (0.645g, 2.69 mmol) in i-PrOH (20 mL). After 5 min, H2O (50 mL) was added and the product was extracted with CH2Cl2 (2 × 50 mL). The organic layers were combined, washed with H2O (2 × 20 mL), dried(Na2SO4), and concentrated. The residue was purified by flash chromatography[silica gel, hexane-benzene (1:1); Rf = 0.15] to give a yellow solid; yield: 0.40 g (44%); mp 71.5-73.5 C.IR (KBr): 3364 (NH) cm-1.1H NMR (300 MHz, CDCl3): delta = 1.28 (t, J = 7.2 Hz, 6 H, 2 × CH3),2.58 (s, 3 H, SCH3), 3.61 (dq, 2J = 9.3 Hz, 3J = 7.2 Hz, 2 H,2 × CHAHBCH3), 3.73-3.85 (m, 4 H, NCH2 and 2 × CHAHBCH3),4.69 (t, J = 5.4 Hz, 1 H, OCH), 8.17 (br s, 1 H, NH).13C NMR (75 MHz, DMSO-d6): delta = 14.5, 15.7, 44.3, 62.3, 99.8,124.6, 152.6, 154.6, 173.0.Anal. Calcd for C11H17ClN4O4S: C, 39.23; H, 5.09. Found: C,39.21; H, 5.07.

The synthetic route of 645-36-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Juskenas, Robertas; Masevicius, Viktoras; Tumkevicius, Sigitas; Synthesis; vol. 45; 17; (2013); p. 2438 – 2446;,
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Some common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, molecular formula is C6H15NO2, 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. HPLC of Formula: C6H15NO2

[00114] To a glass reactor was charged 3,5-dichlorobenzaldehyde. Absolute ethanol was added to the batch slowly (this addition is mildly exothermic) and agitation started. 2,2- Diethoxyethylamine (1.03 equiv) was slowly added to the batch, keeping the batch temperature at 20-78 C. The batch was then heated to 76-78 C for 2 h. GC-MS analysis indicated reactioncompletion (starting material < 1%). The batch was cooled to ambient temperature for work-up. The batch was concentrated in vacuo to a residue and azeotroped with heptanes (x2). The residue was cooled and held at 0-5 C for 12 h to form a suspension. The solids were collected by filtration and the cake was washed with cold (0-5 C) heptanes, and dried under hot nitrogen (45-5 0 C) to afford Compound 2? as a white solid (94% yield). These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 645-36-3, its application will become more common. Reference:
Patent; SARCODE BIOSCIENCE INC.; ZELLER, James, Robert; VENKATRAMAN, Sripathy; BROT, Elisabeth, C.A.; IYER, Subashree; HALL, Michael; WO2014/18748; (2014); A1;,
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Application of 645-36-3, 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. 645-36-3, name is 2,2-Diethoxyethanamine, This compound has unique chemical properties. The synthetic route is as follows.

A solution of the amino-acetaldehyde diethyl acetal (13.16 g, 99 mmol) in ether (35 mL) is added to a suspension of CNBr (10.47 g, 99 mmol) in hexane (35 mL) at room temperature. The reaction mixture is stirred at room temperature overnight. The solid is removed by filtration and washed with ether. The combined filtrate is concentrated. Purification by column chromatography (silica gel, eluding with dichloromethane to 4% methanol in dichloromethane, gradient) affords N-(2,2-Diethoxyethyl)carbodiimide (Rf: 2.70, 4% methanol in dichloromethane, stain with 10% ethanolic molybdatophosphoric acid): 1H NMR 400 MHz (CDCl3) delta 4.58 (t, J=5.2 Hz, 1H), 3.77-3.69 (m, 2H), 3.65 (br, s, 1H), 3.60-3.52 (m, 2H), 3.16 (t, J=5.6 Hz, 1H), 1.23 (t, 6H, J=6.8 Hz).

The chemical industry reduces the impact on the environment during synthesis 2,2-Diethoxyethanamine. I believe this compound will play a more active role in future production and life.

Reference:
Patent; IRM LLC; US2008/188483; (2008); A1;,
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Electric Literature of 645-36-3, A common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, molecular formula is C6H15NO2, 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.

In the three-necked flask has been added9.94 g of aminoacetaldehyde diethyl acetal (0.074 mol)20.6 g of S-methylisothiourea sulfate (0. 074 mol) and 16. 5 ml of water, and then warmed to 110 C. After stirring for 1. 5 h, the reaction was stopped. The solvent was distilled off, followed by addition of 13. 0 g of 37% hydrochloric acid (mass percent, the same as in the following examples) to the reaction solution, stirred at 65 C for 1 h, 50 ml of water was added, the solvent was evaporated, 30 ml of acetone was added to precipitate pale yellow crystals The The crude product was recrystallized from 30 ml of ethanol-water,The resulting white powdery solid 2-aminoimidazolyl sulfate 15. 90 g, yield 81. 5%

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Yancheng Institute Of Technology; Zhao, LingLing; Dai, Yong; Qi, gang; (5 pag.)CN103396369; (2016); B;,
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Electric Literature of 645-36-3, 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. 645-36-3, name is 2,2-Diethoxyethanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Preparation 26; 5-Chloro-thiophene-2-carboxylic acid (2,2-diethoxyethyl) amide; Add 5-chlorothiophene-2-carboxylic acid (100 g, 0.60 mol) and dichloromethane (1000 mL) to a 3 L three-necked round bottom flask equipped with an overhead stirrer, nitrogen inlet/outlet, addition funnel, and thermocouple. Stir the resulting solution under nitrogen while cooling to 4 0C. Add via addition funnel 2,2-diethyoxyethylamine (88.5 ml, 0.60 mol) in dichloromethane (35 mL) over 12 minutes. Add l-(3- dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (123 g, 0.64 mol) to the chilled mixture. Add additional dichloromethane (165 mL) and stir the reaction mixture for 22 h at room temperature. Quench the reaction with water (1000 mL) and separate the resulting layers. Back extract the aqueous layer with dichloromethane (500 mL) and combine the organic layers. Dry over sodium sulfate and purify through a silica gel bed eluting with dichloromethane followed by a mixture of 1% MeOH in dichloromethane and then a mixture of 10% MeOH in dichloromethane to afford 108 g (65%) of the title compound as a white solid. 1H NMR (500 MHz, CDCl3): delta 7.26 (d, J= 3.5 Hz, IH), 6.85 (d, J= 3.5 Hz, IH), 6.37 (bs, IH), 4.57 (t, J= 5.5 Hz, IH), 3.68-3.74 (m, 2H), 3.48-3.57 (m, 4H), 1.19 (t, J= 7.5 Hz, 6H).

The synthetic route of 2,2-Diethoxyethanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; WO2007/146758; (2007); A2;,
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Some common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, molecular formula is C6H15NO2, 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. HPLC of Formula: C6H15NO2

2,2-Diethoxyethylamine (470 muL, 3.23 mmol) was added to a suspension of pyrimidine 9 (0.63 g, 2.67 mmol) in i-PrOH (30 mL), and the mixture was stirred at r.t. until the starting compound has dissolved. Et3N (560 muL, 4.0 mmol) was then added and the mixture was stirred for a further 45 min. H2O (50 mL) was added and the product was extracted with CH2Cl2 (2 × 50 mL). The organic layers were combined, washed with H2O (2 × 20 mL), dried (Na2SO4), and concentrated. The residue was purified by flash chromatography(silica gel, CH2Cl2; Rf = 0.42) to give a yellow solid; yield: 0.61 g(69%); mp 65.5-67.5 C.IR (KBr): 3380 (NH) cm-1. 1H NMR (300 MHz, CDCl3): delta = 1.27 (t, J = 6.9 Hz, 6 H, 2 × CH3),2.55 (s, 3 H, SCH3), 3.60 (dq, 2J = 9.3 Hz, 3J = 6.9 Hz, 2 H,2 × CHAHBCH3), 3.72-3.83 (m, 4 H, NCH2 and 2 × CHAHBCH3),4.09 (s, 3 H, OCH3), 4.68 (t, J = 5.4 Hz, 1 H, OCH), 8.84 (br s, 1 H,NH).13C NMR (75 MHz, CDCl3): delta = 14.8, 15.6, 44.3, 55.7, 63.2, 100.5,113.5, 156.6, 163.8, 174.6.Anal. Calcd for C12H20N4O5S: C, 43.36; H, 6.07. Found: C, 43.68;H, 6.11.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 645-36-3, its application will become more common.

Reference:
Article; Juskenas, Robertas; Masevicius, Viktoras; Tumkevicius, Sigitas; Synthesis; vol. 45; 17; (2013); p. 2438 – 2446;,
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Electric Literature of 645-36-3, 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 645-36-3 as follows.

N- (2-chloropyridine-4-substituted) -4-fluorobenzamide (5g, 19.9mmol) was dissolved in toluene (50mL), cooled to 0 C, and dichlorosulfoxide was slowly added dropwise under nitrogen protection. (7.1 g, 59.8 mmol), transferred to room temperature for 1 hour, and then refluxed overnight. TLC monitoring. After the reaction was completed, the solvent and dichlorosulfoxide were removed to obtain (Z) -N- (2-chloropyridine-4-substituted) -4-fluorobenzimidyl chloride.Dissolve aminoacetaldehyde diethanol (3.5 g, 23.9 mmol) and TEA (4.0 g, 39.8 mmol) in dichloromethane (100 mL), cool to 0 C, and obtain (Z) -N- (2-chloropyridine-4-substituted) -4-fluorobenzimidyl chloride was dissolved in dichloromethane (100 mL), and the solution was slowly added dropwise. The mixture was naturally warmed to room temperature and stirred overnight. Monitored by TLC. After the reaction was completed, the mixture was washed with a saturated ammonium chloride aqueous solution and a saturated saline solution, dried over anhydrous Na2SO4, filtered, and dried. Purification by silica gel column chromatography gave a yellow solid (7 g, 95.7%).

According to the analysis of related databases, 645-36-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Southern Medical University; Zhang Jiajie; Yang Haikui; Wu Shaoyu; Tian Yuanxin; Wan Shanhe; Zhang Tingting; Wu Xiaoyun; Li Zhonghuang; Jiang Ying; Yan Ruohong; Zhu Zhengguang; Hu Xiang; (75 pag.)CN110041302; (2019); A;,
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Reference of 645-36-3,Some common heterocyclic compound, 645-36-3, name is 2,2-Diethoxyethanamine, molecular formula is C6H15NO2, 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 solution of 35 g of P8 in 354 ml of MeOH (methanol) was added 3.5 ml of AcOH (acetic acid). The solution was mixed with 33 ml of aminoacetaldehyde diethylacetal at room temperature and stirred for 3-4 hrs. After the solution was cooled to 10 s C, 3.3 g of the reducing agent NaBH4 (sodiumborohydride) was slowly added thereto. At this time, care had to be taken because of hydrogen gas generation and exothermal reaction. The solution was stirred at room temperature for 1 hr. When the reaction was completed, 354 ml of EA (ethylacetate) and 354 ml of distilled water were added so as to separate layers. The organic layer thus formed was dried over 141 g of MgSO4 (magnesium sulfate) and crystallized in hexane to afford 85 g of P7 as a yellowish solid (yield 80%) . 1H NMR (500MHz, CDCl3), delta 8.36 (d, J=4.8 Hz, IH), delta 7.61 (s, IH), delta 7.17 (d, J=4.2 Hz, IH), delta 7.10 (d, J=4.2 Hz, IH), delta 4.58 (t, J=3.3, IH), delta 4.21 (s, 3H), delta 4.07 (s, 3H), delta 3.68 (m, 2H), delta 3.51 (m, 2H), delta 2.82 (d, J=3.3 Hz, 2H), delta 2.48 (s, 3H), delta 1.19 (t, J=4.2 Hz, 6H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,2-Diethoxyethanamine, its application will become more common.

Reference:
Patent; CHOONGWAE PHARMA CORPORATION; WO2010/120112; (2010); A2;,
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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. 645-36-3, name is 2,2-Diethoxyethanamine, A new synthetic method of this compound is introduced below., category: ethers-buliding-blocks

1.5 g of 2-piperidone was dissolved in 75 mL of mesitylene, 248 muL of titanium tetrachloride was added thereto, and heated at 140C. A solution obtained by dissolving 4.02 g of aminoacetoaldehyde diethyl acetal to 45 mL of mesitylene was prepared, and was added dropwise to the previous mesitylene solution over 3 hours. The mixture was stirred at 140C for 70 hours, then cooled back to room temperature, and was extracted with a 2N aqueous solution of hydrochloric acid. The obtained aqueous layer was basified with a 5N aqueous solution of sodium hydroxide, and then was extracted with chloroform. The organic layer was washed with saturated brine, and then dried over anhydrous sodium sulfate. The insolubles were filtered, the filtrate was concentrated under reduced pressure, and then the purification was carried out by distillation under reduced pressure (3mmHg, 120C), to obtain 375 mg of 5,6,7,8-tetrahydroimidazo[1,2-a]pyridine [44-1] as a pale yellow oily product.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; BANYU PHARMACEUTICAL CO., LTD.; EP1790650; (2007); A1;,
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Ether | (C2H5)2O – PubChem