Month: May 2021

Related Products of 18014-00-1, A common heterocyclic compound, 18014-00-1, name is Dimethyl 2,5-dibromoterephthalate, molecular formula is C10H8Br2O4, 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 15 mL vial tube equipped with a magnetic stirring bar and a teflon screw cap were addeddimethyl 2,5-dibromoterephthalate (0.28 g, 0.8 mmol),1) N-methylaniline derivative (8.0 mmol),Pd2(dba)3 (34 mg, 0.06 mmol), RuPhos (70 mg, 0.24 mmol), K3PO4 (1.70 g, 8.0 mmol), and toluene(3.2 mL) under argon atmosphere. The mixture was stirred at 100 C for 10 h. The resultingmixture was allowed to cool to room temperature, and CH2Cl2 (10 mL) was added to the vial. Theprecipitate was removed by suction filtration and the filtrate was concentrated by evaporation underreduced pressure. The crude product was purified by column chromatography on silica gel(hexane/CH2Cl2 2:1 to 1:1) to give 1.

The synthetic route of 18014-00-1 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Shimizu, Masaki; Asai, Yuiga; Takeda, Youhei; Yamatani, Akinori; Hiyama, Tamejiro; Tetrahedron Letters; vol. 52; 32; (2011); p. 4084 – 4089;,
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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. 25415-67-2, name is Ethyl 4-methylpentanoate, A new synthetic method of this compound is introduced below., Application In Synthesis of Ethyl 4-methylpentanoate

REFERENCE EXAMPLE 11 Ethyl 2-(4-bromophenylacetyl)-4-methyl-3-oxopentanoate To a suspension of NaH (7.6 g, 158 mmol) in toluene (142 mL) at 0 C. was added dropwise a solution of ethyl isobutylylacetate (20 g, 126 mmol) in toluene (52 mL) and the resulting solution was stirred under an argon atmosphere for 30 min. Then, a solution of 4-bromophenylacetyl chloride (29.4 g, 126 mmol, prepared as described in reference example 1) in toluene (98 mL) was slowly added and the reaction mixture stirred at room temperature overnight. The resulting solution was poured into H2 O-EtOAc and extracted with H2 O (2*). The organic phase was washed with brine, the aqueous phase was acidified and extracted with EtOAc, and the combined organic phases were dried and concentrated. The residue was chromatographed on silica gel (hexane-EtOAc, 5%) to afford the title compound (29 g, 65%). 1 H-NMR-(CDCl3) delta (TMS): 1.16 (d, J=6.4 Hz, 6H), 1.31 (t, J=7.2 Hz, 3H), 3.09 (q, J=6.4 Hz, 1H), 3.87 (s, 2H), 4.26 (q, J=7.2 Hz, 2H), 7.12 (d, J=8 Hz, 2H), 7.41 (d, J=8 Hz, 2H), 17.49 (s, 1H).

The synthetic route of 25415-67-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; J. Uriach & Cia, S.A.; US5827863; (1998); A;,
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Related Products of 2171-74-6, A common heterocyclic compound, 2171-74-6, name is Benzo[d][1,3]dioxol-2-one, molecular formula is C7H4O3, 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.

Molar ratio between the reagents PCC:ethanol = 1:6.In a two-neck flask 520 jil of ethanol, the basic catalyst (sodium methoxide, in a molar ratio of 1 to 30 with respect to the PCC, 0.003 g),and in the end the PCC (0.201g) are initially added.Subsequently, the flask is equipped with two condensers, rinsed and placed in inert nitrogen atmosphere (refrigerants closed at the ends by suitable caps) and heated, in an oil bath and under magnetic stirring, at the temperature of 60C for one hour.After the reaction, the mixture is rapidly cooled to room temperature and the whole is recovered and solubilized in 10 ml of HPLC acetone. 10 il of decane as an internal standard for the analysis are then added.Gas chromatographic analysis was performed with a Focus-GC instrument model of Thermo, equipped with a HP-5 capillary column anda FID detector.The desired product (DEC) is obtained with a gas chromatographic yield of 93% with a total conversion of the limiting reagent (PCC), without any substantial trace of undesired products, beside the catechol (co-product of the reaction).

The synthetic route of 2171-74-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ALMA MATER STUDIORUM – UNIVERSITA DI BOLOGNA; UNIVERSITA CA’ FOSCARI; TABANELLI, Tommaso; CAVANI, Fabrizio; SELVA, Maurizio; (37 pag.)WO2017/51363; (2017); A1;,
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Application of 87661-20-9,Some common heterocyclic compound, 87661-20-9, name is tert-Butyl cyclopropanecarboxylate, molecular formula is C8H14O2, 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.

Step 1: A solution of n-butyl lithium in hexane (1.4M, 95.7 mL, 0.13 mol) was added drop wise to a solution of freshly distilled diisopropylamine (18.75 mL, 0.12 mol) in dry THF (400 mL) at -60 C. under nitrogen atmosphere. The reaction mixture was slowly warmed to -20 C. and stirred for 30 min. The reaction mixture was re-cooled to -60 C. and cyclopropanecarboxylic acid tert-butyl ester (17.34 g, 0.12 mol) added drop wise over a period 30 min. Reaction mixture was slowly warmed to -20 C. and stirred for 30 min. To the re-cooled (-60 C.) reaction mixture was added drop wise 1,12-dibromododecane (40.0 g, 0.12 mol) in dry THF (40 mL) and DMPU (3.12 g, 0.02 mol). Then the temperature was allowed to reach room temperature and stirred at same temperature over a period of 16 h. The resulting reaction mixture was quenched with saturated NH4Cl (500 mL) at 0 C. and the reaction mixture was extracted with ethyl acetate (400 mL×3). The organic phases were combined, dried over anhydrous Na2SO4 and volatiles were evaporated under reduced pressure to yield a pale yellow liquid which was purified through silica gel (230-400) column (0.5% ethyl acetate in petroleum ether) to give product as pale yellow liquid 14.0 g (29%).1H NMR (300 MHz, DMSO-d6) delta (ppm): 1.55-1.61 (m, 2H), 1.08-1.12 (m, 2H), 1.35 (bs, 13H), 1.49 (bs, 16H), 1.64-1.89 (m, 2H), 3.42 (t, J=6.9 Hz, 2H).

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

Reference:
Patent; KAREUS THERAPEUTICS, SA; US2012/71528; (2012); 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. 18014-00-1, name is Dimethyl 2,5-dibromoterephthalate, A new synthetic method of this compound is introduced below., Formula: C10H8Br2O4

210 mg of 4-fluorothiopheneboronic acid, 170 mg of dimethyl 2,5-dibromobenzene-1,4-dicarboxylate,116mg PdCl2 (MeCN) 2, 336mg saturated K2CO3 aqueous solution was placed in a two-port bottle,Add 12 mL of tetrahydrofuran,The mixture was heated and stirred under reflux for 7 hours under argon.After cooling to room temperature, it was extracted with 30 mL of diethyl ether.The combined organic layers were washed with saturated brine andNa2SO4 is dry.The solution was then filtered and the solvent removed to give a crude material which was crystallised from ethanol.The product was obtained as a yellow solid. A mixture of 500 mg of yellow solid in 20 mL of ethanol and 286 mg of NaOH was refluxed for 7 h.After cooling to room temperature, the mixture was poured into hydrochloric acid.A yellow solid product was obtained by suction filtration.The yellow solid was mixed with 50 mL of polyphosphoric acid, and the mixture was stirred at 130 C for 3 hours and then washed with ice water. A black solid crude product was obtained by suction filtration.The obtained crude product was recrystallized from dimethylformamide to give a final product with a metallic luster.

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; Lanzhou University; Zhang Haoli; Liu Duanwu; Lin Zewei; Xu Zhuguo; Shi Zifa; (13 pag.)CN109678877; (2019); A;,
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Application of 143165-48-4, 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. 143165-48-4, name is Ethyl 2-(3-chloropropoxy)acetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

RF = 0.33 (cyclohexane/ethyl acetate 8:2). The 3-iodo-propoxy-acetic acid ethyl ester was prepared in analogy to Example 4 d) from 3-cloro-propoxy-acetic acid ethyl ester (Suomen Kemistilehti 17 B, 17 (1944), cf. CA 40, 6491 (1946)). Boiling point0.65: 85C.

The synthetic route of Ethyl 2-(3-chloropropoxy)acetate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hoechst Aktiengesellschaft; US3984459; (1976); A;,
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Some common heterocyclic compound, 915213-54-6, name is Ethyl 2-(4,4-difluorocyclohexyl)acetate, molecular formula is C10H16F2O2, 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. category: esters-buliding-blocks

To a solution of ethyl 2-(4-oxocyclohexyl)acetate (0.4 g) in DCM (5 mL) was added Deoxo-Fluor (0.881 mL) and EtOH (0.038 mL). The reaction mixture was stirred at rt for 16 h and then diluted with sat. aHC03 and EtOAc. The organic phase was washed with water, sat. NaCl and dried over anhydrous Na2S04, filtered and dried to yield ethyl 2-(4,4-difluorocyclohexyl)acetate (0.4 g). To a solution of ethyl 2-(4,4-difluorocyclohexyl) acetate in THF/MeOH (2 mL) was added IN NaOH (1 mL), and the reaction mixture was stirred at rt for 16 h. The reaction mixture was concentrated, then diluted with EtOAc and acidified with IN HCl. The organic phase was washed with sat. NaCl, dried over anhydrous Na2S04, filtered and concentrated to yield 2-(4,4-difluorocyclohexyl)acetic acid as a yellow solid. 1H NMR (400 MHz, DMSO-i) ppm 12.13 (1 H, br. s.), 2.06 – 2.28 (3 H, m), 1.92 – 2.03 (1 H, m), 1.72 – 1.91 (4 H, m), 1.31 – 1.48 (1 H, m), 1.10 – 1.31 (2 H, m).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 915213-54-6, its application will become more common.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; HEWAWASAM, Piyasena; LOPEZ, Omar D.; TU, Yong; WANG, Alan Xiangdong; XU, Ningning; KADOW, John F.; MEANWELL, Nicholas A.; GUPTA, Samayamunthula Venkata Satya Arun Kumar; KUMAR, Indasi J. Gopi; PUNUGUPATI, Suresh Kumar; BELEMA, Makonen; WO2015/5901; (2015); A1;,
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These common heterocyclic compound, 29006-01-7, name is Methyl 4-methoxybutanoate, 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. Recommanded Product: 29006-01-7

Example 25 A solution of methyl 4-methoxybutanoate (1.0 g, 7.57 mmol) in THF (20 mL) was treated with a solution of LiOH (0.362 g, 15.13 mmol) in H2O (5 mL) and stirred at RT for 16 h. The mixture was concentrated to dryness, acidified with 2M HCl, diluted with H2O, extracted with EtOAc (2×) and the combined organics were washed with brine, dried over Na2SO4 and concentrated to dryness to afford 4-methoxybutanoic acid (860 mg, 96%) as a viscous oil. 1H NMR (400 MHz, DMSO-d6): delta 12.02 (s, 1H), 3.28 (t, J=6.4 Hz, 2H), 3.19 (s, 3H), 2.21 (t, J=7.4 Hz, 2H), 1.69 (m, 2H).

The synthetic route of Methyl 4-methoxybutanoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Deciphera Pharmaceuticals, LLC; Flynn, Daniel L.; Caldwell, Timothy Malcolm; Kaufman, Michael D.; Patt, William C.; Samarakoon, Thiwanka; Vogeti, Lakshminarayana; Yates, Karen M.; US2014/275080; (2014); A1;,
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Synthetic Route of 85920-63-4, These common heterocyclic compound, 85920-63-4, name is 5-(1-Hydroxyethylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione, 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.

Enaminone 15 (3.0 g, 15.7 mmol, 1.0 equiv.) and freshly ground acyl Meldrum’s acid (8.76 g, 47.1 mmol, 3.0 equiv.) were dissolved in toluene (157 mL) and the solution was heated to reflux for 45 min. Removal of the volatiles yielded a brown semisolid. The crude material was purified using acidified silica gel* and 7:1 hexanes: ethyl acetate as the eluent to afford 14 as a white solid (1.55?g, 6.73?mmol, 43%).

The synthetic route of 85920-63-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Eliasen, Anders M.; Chin, Matthew R.; Axelrod, Abram J.; Abagyan, Ruben; Siegel, Dionicio; Tetrahedron; vol. 74; 26; (2018); p. 3238 – 3245;,
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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. 146307-51-9, name is trans-Methyl 4-((tert-butoxycarbonyl)amino)cyclohexanecarboxylate, This compound has unique chemical properties. The synthetic route is as follows., name: trans-Methyl 4-((tert-butoxycarbonyl)amino)cyclohexanecarboxylate

Step 2: Trans-tert-butyl 4-(hydroxymethyl)cyclohexylcarbamateMethyl trans-4-(tert-butoxycarbonylamino)cyclohexanecarboxylate (55.5 g, 216 mmol) was suspended in ethanol (900 ml) and THF (100 ml) and the mixture was cooled to 5C. Granular calcium chloride (47.9g, 431 mmol) was added portionwise to give a milky suspension. Sodium borohydride (32.6 g, 863 mmol) was added portionwise over 25 mins at 5C. The reaction mixture (white emulsion) was stirred at 5C for 1 hour, the water bath was removed and then the reaction mixture was allowed to warm to room temperature and stirred at room temperature overnight. The reaction mixture was cooled to 10C and 5% potassium carbonate (200 ml) was added dropwise until the pH of the solution was pH11. A colourless precipitate formed which was filtered off. The solid was stirred with ethyl acetate (2000 ml) and water (500 ml). The organic layer was separated and washed with 0.5M HCI (200 ml), then washed with water (2 x 200 ml) and saturated brine (100 ml). The organic solution was dried over anhydrous MgS04, filtered and evaporated to give a white solid The solid was dried under high vacuum overnight to constant weight; [M+H]+230.

According to the analysis of related databases, 146307-51-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ATKINSON Benjamin; BEATTIE David; CULSHAW Andrew James; DEVEREUX Nicholas James; MCKENNA Jeffrey; DALE James; WO2011/92293; A1; (2011);,
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