Month: May 2021

Reference of 59227-79-1,Some common heterocyclic compound, 59227-79-1, name is Ethyl 4-(4-chlorophenoxy)butanoate, molecular formula is C12H15ClO3, 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: Hydrazine hydrate (0.045 mol) was added to the solution of compounds 3a-l (0.03 mol) in ethanol (20 ml) and stirred the reaction mixture at room temperature for 5 h. Reaction completion was monitored by thin layer chromatography using hexane:ethylacetate (2:1) as the mobile phase and allowed to stand overnight. The white crystals 4a-l formed were filtered, washed and after drying recrystallized from ethanol. 4-(4-Chloro-phenoxy)-butyric acid hydrazide (4b) Yield 90%; mp 85-87 C; FT-IR (KBr, cm-1): 3315 (NH2), 3220 (NH), 1672 (C=O); 1H NMR (CDCl3): delta 2.26 (m, 2H, CH2), 2.75 (t, 2H, COCH2), 3.85 (d, 2H, NH2), 4.07 (t, 2H, OCH2), 6.88 (d, J = 8.80 Hz, 2H, Ar-H), 7.27 (d, J = 8.85 Hz, 2H, Ar-H), 8.40 (t, 1H, NH); LC-MS m/z 229 (M + 1). Anal. Calcd. for C10H13ClN2O2: C, 52.52; H, 5.73; N, 12.25. Found: C, 52.43; H, 5.75; N, 12.39%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 4-(4-chlorophenoxy)butanoate, its application will become more common.

Reference:
Article; Al-Ghorbani, Mohammed; Vigneshwaran; Ranganatha, V. Lakshmi; Prabhakar; Khanum, Shaukath Ara; Bioorganic Chemistry; vol. 60; (2015); p. 136 – 146;,
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Some common heterocyclic compound, 22286-82-4, name is Ethyl 2-phenylacrylate, molecular formula is C11H12O2, 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. Product Details of 22286-82-4

EXAMPLE 1 1-(2-Chlorophenyl)-4,5-dihydro-2[2-(imidazol-1-yl)-1-phenylethyl]imidazole A solution of ethyl 2-phenylprop-2-enoate (160 g, 0.45 mol), imidazole (36.7 g 0.54 mol) and tetramethylguanidine (2 g, 0.017 mol) in dry tetrahydrofuran (1 L) was heated at reflux temperature for 3 hours. The solvent was removed under reduced pressure and the residue was dissolved in dilute hydrochloric acid. The resulting aqueous solution was washed with ether, basified with dilute aqueous sodium hydroxide and extracted with chloroform. The organic phase was separated, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to yield ethyl 3-(imidazol-1-yl)-2-phenylpropanoate (90 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 22286-82-4, its application will become more common.

Reference:
Patent; G. D. Searle & Co.; US4661602; (1987); A;,
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Electric Literature of 1731-79-9,Some common heterocyclic compound, 1731-79-9, name is Dimethyl dodecanedioate, molecular formula is C14H26O4, 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: Into a reaction flask dicarboxylic acid dimethyl ester and fatty alcohol or cholesterol were added at the ratio of 1:2, respectively. After addition of the ionic liquid catalyst (2.5 mmol %) the resulting mixture was heated with stirring at 110 C for 16 h. At the end of this, the flask was cooled to room temperature and the resulting solid reaction mixture was crystallized from THF/MeOH to afford pure crystalline product.

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

Reference:
Article; Yildirim, Ayhan; Kiraylar, Kaan; Turkish Journal of Chemistry; vol. 43; 3; (2019); p. 802 – 808;,
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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. 123-95-5, name is Butyl stearate, This compound has unique chemical properties. The synthetic route is as follows., category: esters-buliding-blocks

An esterification reaction mixture (94 g), consisting of butanol (ca., 4.9% w/w), butyl stearate (95.1% w/w), residual stearic acid (trace), residual methanesulfonic acid catalyst (1383 ppm) and undesired butyl methanesulfonate (613 ppm) was treated with 45% aqueous KOH (229 mg, 1.84 mmol as compared to 1.74 mmol MSA originally charged to the reaction). The resulting mixture was heating at 50 C. for 40 minutes. Without wishing to be bound by any particular theory or explanation, it is believed that reaction of butyl stearate with KOH produced potassium stearate, which retains significant solubility in the butyl stearate medium. The formed potassium stearate then reacted with butyl methanesulfonate to produce potassium methanesulfonate and butyl stearate. After filtration of the by-product solid salts (0.6325 g), analysis of the mixture by gas chromatography revealed only 300 ppm unreacted butyl methanesulfonate, a 51% reduction. Repetition of the above KOH treatment at a higher temperature (175 C./60 min.) revealed complete reaction of the butyl methanesulfonate. Similarly, treatment with NaOH was found equally effective as treatment with KOH. Treatment with Ca(OH)2 proved ineffective, presumably due to formation of poorly soluble calcium salts. Treatment with acidic tin(II) or zirconium (IV) salts resulted in formation of additional butyl methanesulfonate.

According to the analysis of related databases, 123-95-5, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Smith, Gary; Cordova, Robert; Chen, Johnson C.H.; Chen, Mabel; US2006/30725; (2006); A1;,
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Related Products of 32864-38-3,Some common heterocyclic compound, 32864-38-3, name is tert-Butyl ethyl malonate, molecular formula is C9H16O4, 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 stirred solution of S3 (1.88 g, 10 mmol) in 30 mL of MeCN at 0 °C was added p-ABSA (3.6 g, 15 mmol) andEt3N (4.2 mL, 30 mmmol). After stirring the reaction mixture at 0 °C 1 h, the mixture was warmed up to rt andstirred for 13 h. The mixture was filtered through a pad of Celite and the filtrate was concentrated in vacuo. Thecrude product was purified by silica gel column chromatography (nhexane/AcOEt = 15/1) to give the titlecompound (1.93 g, 90percent) as a pale yellow oil.

The synthetic route of 32864-38-3 has been constantly updated, and we look forward to future research findings.

Reference:
Article; March, Taryn; Murata, Akihiro; Kobayashi, Yusuke; Takemoto, Yoshiji; Synlett; vol. 28; 11; (2017); p. 1295 – 1299;,
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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. 2459-25-8, name is Methyl 2-naphthoate, A new synthetic method of this compound is introduced below., Formula: C12H10O2

Under a nitrogen atmosphere,Dissolve 50 g of methyl naphthalene-2-carboxylate in 350 mL of tetrahydrofuran.In a three-necked flask, the temperature of the system was reduced to -10C with liquid nitrogen.A 2mol/L solution of lithium diisopropylamide in tetrahydrofuran was added to the reaction system, wherein the volume of lithium diisopropylamide was 173.6mL, and then the temperature was raised to 20C and kept warm for 3 hours and then lowered to -80C and 87g was added. 1,2-Dibromoethane was reacted at -80C for 0.5 h, then allowed to stand at room temperature. The reaction solution was poured into a mixture of 500 mL of ethyl acetate and 2000 mL of a 10% volume aqueous solution of hydrochloric acid.After stirring for 10 minutes, let stand for 0.5h and discard the lower aqueous phase.The organic layer obtained from the upper layer was dried with 40 g of anhydrous sodium sulfate for 0.5 h.After filtration, the filtrate was distilled under reduced pressure at 45 C and -0.08 MPa until no solvent flowed out.The crude product of 3-bromonaphthalene-2-carboxylic acid methyl ester was obtained 69 g ,The crude product was added to 517 mL of ethanol and heated to reflux at 45 C. for 2 h.Then it was cooled to 0C for 1 h, filtered, and the filter cake was dried at 50C for 2 h.Obtained 66.5 g of 3-bromonaphthalene-2-carboxylic acid methyl ester, yield 93.5%, purity >98%.

The synthetic route of 2459-25-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shanxi Laite Optoelectric Materials Co., Ltd.; Liu Ruigang; Zhang Wen; Li Jian; Li Lingang; Xue Zhen; Wang Yalong; (7 pag.)CN107602381; (2018); A;,
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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. 87661-20-9, name is tert-Butyl cyclopropanecarboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of tert-Butyl cyclopropanecarboxylate

15.9 ml (1.15 equiv.) diisopropylamine were dissolved in 65 ml tetrahydrofuran and cooled to ca -10 C. 65 ml (1.08 equiv.) 1.6 M butyllithium solution in hexane were added over 25 min, maintaining the temperature between -10 C. and 0 C. After 50 nm in at ca. -5 C., the reaction mixture was cooled to -75 C. A solution of 15 g (96.7 mmol, 1 equiv., 92% w/w purity) cyclopropanecarboxylic acid tert-butyl ester in 20 ml tetrahydrofuran was added over 15 min keeping the temperature between -75 C. and -70 C. The reaction mixture was stirred 5 h at -75 C. (milky reaction mixture obtained after 2.5 h). A solution of 12.87 g (1.10 equiv.) allyl bromide was added over 20 min keeping the temperature between -75 C. and -60 C. The reaction mixture was stirred at -78 C. for 1 h, warmed to room temperature and stirred overnight. The reaction mixture was cooled to 0 C. 100 ml sat. aq. ammonium chloride solution were added followed by 30 ml water providing a clear biphasic mixture. The mixture was extracted 3 times with 50 ml tert-butyl methyl ether. The organic phases were combined, dried over sodium sulfate, filtered and concentrated under reduced pressure (40 C./20 mbar) to afford 16.44 g of crude product. The crude product was distilled (2 mbar; ca 40 C. distillation head temperature) to provide the title compound in ca 65% yield.

The synthetic route of 87661-20-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Aebi, Johannes; Binggeli, Alfred; Green, Luke; Hartmann, Guido; Maerki, Hans P.; Mattei, Patrizio; Ricklin, Fabienne; US2009/23713; (2009); A1;,
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Synthetic Route of 80051-07-6, These common heterocyclic compound, 80051-07-6, name is Methyl 4-(1-aminoethyl)benzoate, 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 a stirred solution ofthe corresponding amine (2 mmol) in anhydrous CH2Cl2 containing drytriethylamine (5 mmol) a solution of 3 or 15a-c (2.5 mmol) in anhydrousCH2Cl2 (5 mL) was added dropwise over 15 min at 0 C. Afterstirred for another 5 h at room temperature, water was added, and themixture was extracted with CH2Cl2. The combined organic phase wasdried (Na2SO4) and filtered to obtain the crude products, which werepurified by column chromatography using silica gel and a CH2Cl2/MeOH mixture. (CH2Cl2: MeOH=100:1)

Statistics shows that Methyl 4-(1-aminoethyl)benzoate is playing an increasingly important role. we look forward to future research findings about 80051-07-6.

Reference:
Article; Hu, Jinhui; An, Baijiao; Pan, Tingting; Li, Zhengcunxiao; Huang, Ling; Li, Xingshu; Bioorganic and Medicinal Chemistry; vol. 26; 21; (2018); p. 5718 – 5729;,
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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. 40637-56-7, name is Dimethyl 2-allylmalonate, A new synthetic method of this compound is introduced below., Application In Synthesis of Dimethyl 2-allylmalonate

General procedure: A 50 mL Schlenk tube containing NaH (60% in mineral oil, 240 mg, 6 mmol)was evacuated and filled with argon (3x). THF (10 mL) was added and thesuspension was cooled in ice/water bath. Appropriately substituted dimethyl(allyl)malonate (5 mmol) was added dropwise (caution, hydrogen evolution),then cooling bath was removed and the reaction mixture was stirred at rt for 30min. Then substituted propargil bromide or methanesulfonate (6 mmol) wasadded and the reaction mixture was stirred at rt for 1h. The mixture wasquenched with NH4Cl(aq.) (20 mL) and extracted with MTBE (3 × 20 mL). Combined organic extractswere dried (Na2SO4), concentrated and crude product was purified by column chromatography onsilica gel (50 g column, 98:2 ? 95:5 hexanes/EtOAc).

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:
Article; Kocoj, Ma?gorzata; Jarosi?ska, El?bieta; Cha?adaj, Wojciech; Synlett; vol. 29; 10; (2018); p. 1319 – 1323;,
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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. 2672-58-4, name is Trimethyl benzene-1,3,5-tricarboxylate, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 2672-58-4

Synthesis of 1,3,5-Tris(hydroxymethyl)benzene (50)(Y. Yamaqiwa, Y. Koreishi. S. Kivozumi, M. Kobavashi, T. Kamikawa, M. Tsukino, H. Goi M. Yamamaoto, M. Munakata. Bull. Chem. Soc. Jpn. 1996, 69, 3317-3323; J. Houk, G. Whitesides. J. Am. Chem. Soc. 1987, 109, 6825-6836) A solution of 1,3,5-tris(methoxycarbonyl)benzene (10.09 g, 40 mmol) in dry THF (400 ml) was added over a period of 3h to a suspension of LiAlH4 (4.03 g, 0.1 mol) in dry THF (300 ml) under N2. After stirring over night at room temperature, the reaction mixture was cooled to 0 C., hydrolyzed with water (4 ml), 2M NaOH (4 ml) and water (12 ml), filtered, and the filter cake washed thoroughly with THF. The combined filtrates were concentrated and the crude product was recrystallized from hot (not boiling) ethanol to afford 50(5.59 g, 83%) as white needles; mp 76-77 C. (lit. 77-78 C.) 1H NMR (300 MHz, DMSO-d6) delta4.49 (d, 3H, J4.8 Hz, CH2), 5.30 (t, 1H, J5.4 Hz, OH), 7.14 (s, 1H, aromat. H).

According to the analysis of related databases, 2672-58-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Davis, Benjamin G.; Jones, John Bryan; Bott, Richard R.; US2002/19039; (2002); A1;,
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