Day: August 20, 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3663-80-7,2,3-Dihydrobenzo[b][1,4]dioxine-2-carboxylic acid,as a common compound, the synthetic route is as follows.

General procedure: To a solution of 8 (0.2 mmol, 1 equiv) in CH2Cl2 (2 mL) were added NEt3 (0.6 mmol, 3 equiv), N,N,N?,N?-tetramethyl-O-(1H-benzotriazol-1-yl)uronium hexafluorophosphate (HBTU, 0.26 mmol, 1.3 equiv) and the appropriate carboxylic acid (1.25 equiv). The reaction was stirred overnight and then concentrated. The crude material was purified by silica gel column chromatography using a gradient of 0-100percent EtOAc/hexanes.

The synthetic route of 3663-80-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Amato, George S.; Manke, Amruta; Vasukuttan, Vineetha; Wiethe, Robert W.; Snyder, Rodney W.; Runyon, Scott P.; Maitra, Rangan; Bioorganic and Medicinal Chemistry; vol. 26; 15; (2018); p. 4518 – 4531;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4442-54-0,2,3-Dihydro-1,4-benzodioxine-6-carboxylic acid,as a common compound, the synthetic route is as follows.

1. Preparation of ethyl 2-[1-[4-(2,3-dihydrobenzo[b][1,4]dioxin-6-carboxamido)benzyl]-1H-indazol-3-yl]acetate 2,3-Dihydrobenzo[b][1,4]dioxin-6-carboxylic acid (154 mg, 0.85 mmol) was dissolved in dichloromethane (15 mL) and N,N-dimethylformamide (0.10 mL), and in an ice bath, oxalic chloride (162 mg, 1.28 mmol) was added dropwise slowly. Upon completion of the dropwise addition, it was moved to react at room temperature for 3 hours, concentrated under reduce pressure to obtain 2,3-dihydrobenzo[b][1,4]dioxin-6-formyl chloride as a white solid.

4442-54-0 2,3-Dihydro-1,4-benzodioxine-6-carboxylic acid 2758833, abenzodioxans compound, is more and more widely used in various.

Reference£º
Patent; Zhang, Yan; Zhang, Min; Lo, Hoyin; US2014/303186; (2014); A1;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

3663-79-4, Methyl 1,4-Benzodioxane-2-carboxylate is a benzodioxans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: Methyl 1,4-benzodioxan-2-carboxylate (¡À)-17a was dissolved in ? THF/ ? H2O (1:1 ratio) after which ? lithium hydroxide was added. The reaction was stirred for 3?h until hydrolysis was complete. Next, THF was evaporated and the residue acidified with 10percent HCl. DCM was used for extraction. The organic layers were dried in vacuo to give ? (¡À)-1,4-benzodioxan-2-carboxylic acid 1 in 91percent yield as a white solid; mp 117?119?¡ãC; [lit.23b 125.4]; 1H NMR: delta 4.44 (d, J?=?4.8?Hz, 2H), 4.90 (t, J?=?3.7, 7.6?Hz, 1H), 6.88?6.97 (m, 3H), 6.99?7.02 (m, 1H); 13C NMR: delta 64.63, 71.61, 117.34, 122.38, 141.97, 142.87 173.59; HRMS (ESI) Calcd for C9H8NaO4 (M+Na): 203.0320. Found: 203.0317.

The synthetic route of 3663-79-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Rouf, Abdul; Gupta, Pankaj; Aga, Mushtaq A.; Kumar, Brijesh; Chaubey, Asha; Parshad, Rajinder; Taneja, Subhash C.; Tetrahedron Asymmetry; vol. 23; 22-23; (2012); p. 1615 – 1623;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

2879-20-1, 1-(2,3-Dihydrobenzo[b][1,4]dioxin-6-yl)ethanone is a benzodioxans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: Acetophenone 1a (120 mg, 1.0 mmol), pyridine 2a (158 mg, 2.0 mmol), and iodine (254 mg, 1.0 mmol) were placed in an oven-dried and argon filled Schlenk tube. After addition of anhydrous DMSO (5 mL), the mixture was stirred at 100 C for 36 h. After the reaction completed, the mixture was diluted with water and treated with Na2S2O3 (5% w/w, aq) until the color turned to pale yellow. The mixture was then extracted with CH2Cl2 (3¡Á20 mL), the combined organic extracts were dried over Na2SO4 and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel (eluent: CH2Cl2/EtOAc=200:1) to afford a yellow solid 3aa (122 mg, 85%).

2879-20-1 1-(2,3-Dihydrobenzo[b][1,4]dioxin-6-yl)ethanone 76143, abenzodioxans compound, is more and more widely used in various.

Reference£º
Article; Yang, Yan; Gao, Meng; Zhang, Dong-Xue; Wu, Liu-Ming; Shu, Wen-Ming; Wu, An-Xin; Tetrahedron; vol. 68; 36; (2012); p. 7338 – 7344;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.2879-20-1,1-(2,3-Dihydrobenzo[b][1,4]dioxin-6-yl)ethanone,as a common compound, the synthetic route is as follows.

General procedure: A 10 mL glass flask equipped with a magnetic stir bar wascharged with a methyl ketone (1 mmol) and dissolved in MeCN (2 mL). To thethermostated solution NH4NO3 (10-25 mol %), I2 (50 mol %) and H2SO4(aqueous 96% solution, 10-20 mol %) were added and the flask was furtherequipped with a balloon filled with air (1 L) and magnetically stirred at 60 C.The consumption of starting material was monitored by TLC. After completionof the reaction, the mixture was cooled to room temperature, diluted withEtOAc (10 mL), and insoluble material identified as ammonium sulfate wasfiltered off. The filtrate neutralized with NaHCO3 (aqueous 10% solution, 2 mL)and Na2S2O3 (aqueous 10% solution, 2 mL) and phase was separated. The waterphase was washed with EtOAc additionally two times (2 5 mL). The combinedorganic phase was dried over anhydrous Na2SO4 and the solvent distilled underreduced pressure. The crude product obtained was analyzed by 1H NMR. Finallythe crude product was purified using column chromatography (SiO2, n-hexane/CH2Cl2 elution) and preparative thin layer chromatography to afford purematerial, which was compared to authentic samples. Detailed data, concerningcatalyst loading, reaction times, yields of pure products and their spectroscopicand other identification data are given in SI in the chapter Characterization dataof isolated final products. Characterization, for example, 1-(9H-fluoren-2-yl)-2-iodoethanone (2i): 1-(9H-Fluoren-2-yl)ethanone (1 mmol, 208.3 mg), NH4NO3(0.15 mmol, 12 mg), I2 (0.50 mmol, 126.7 mg), H2SO4 (aqueous 96% solution,0.10 mmol, 5.56 lL), 2 mL MeCN, balloon filled with 1 L of air, 60 C, 20 h were used; crystallization from acetone; yield: 187.2 mg (55%) yellow solid, mp 163-164 C. 1H NMR (303 MHz, CDCl3+two drops of DMSO, 25 C, TMS): d (ppm) 3.92 (s,2H), 4.41 (s, 2H), 7.32-7.44 (m, 2H), 7.54-7.59 (m, 1H), 7.77-7.84 (m, 2H), 7.96-8.02(m, 1H), 8.13 (s, 1H); 13C NMR (76.2MHz, CDCl3+two drops of DMSO, 25 C): d(ppm) 2.3, 36.6, 119.6, 120.7, 125.0, 125.3, 126.9, 128.1, 128.1, 131.5, 139.9, 143.2,144.3, 146.8, 192.4;MS (ESI):m/z 335 ((M+H)+, 100%);HR-MS (ESI):m/z = 334.9925,calcd for C15H12IO: 334.9933; Anal. calcd for C15H11IO: C, 53.92; H, 3.32; found: C,54.39; H, 3.05. 3-(2-Iodoacetyl)-2H-chromen-2-one (2o): 3-Acetyl-2H-chromen-2-one (1 mmol, 188.2mg), NH4NO3 (0.20 mmol, 16 mg), I2 (0.50 mmol, 126.7mg),H2SO4 (aqueous 96% solution, 0.1 mmol, 5.56 lL), 2mLMeCN, balloon filledwith 1 Lof air, 60 C, 23 h were used; column chromatography (SiO2, CH2Cl2); yield:182.2mg (58%), yellow solid; mp 135-138 C. 1H NMR (303.0 MHz, CDCl3, 25C,TMS): d (ppm) 4.68 (s, 2H), 7.34-7.46 (m, 2H), 7.64-7.76 (m, 2H), 8.66 (s, 1H); 13CNMR (76.2MHz, CDCl3, 25 C): d (ppm) 6.8, 116.7, 118.1, 121.4, 125.1, 130.2, 134.9,149.5, 155.3, 158.6, 190.1; MS (ESI): m/z 314.9 ((M+H)+, 100%); HR-MS (ESI): m/z = 314.9523, calcd for C11H8IO3: 314.9518.

2879-20-1 1-(2,3-Dihydrobenzo[b][1,4]dioxin-6-yl)ethanone 76143, abenzodioxans compound, is more and more widely used in various.

Reference£º
Article; Prebil, Rok; Stavber, Stojan; Tetrahedron Letters; vol. 55; 41; (2014); p. 5643 – 5647;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

2879-20-1, 1-(2,3-Dihydrobenzo[b][1,4]dioxin-6-yl)ethanone is a benzodioxans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A mixture of acetophenone 4a (120 mg, 1.0 mmol), iodine (254 mg, 1.0 mmol), and CuO (88 mg, 1.1 mmol) in anhydrous methanol (10 mL) was heated at reflux, after disappearance of the reactant (1-12 h, monitored by TLC), 1,2-diamines 2a (108 mg, 1.0 mmol) and K3PO4*3H2O (266 mg, 1.0 mmol) was added and the mixture was stirred for 12 h at 40 C. The solvent was removed under reduced pressure, and 50 mL water was added to mixture, extracted with EtOAc three times (3¡Á50 mL). The extract was washed with Na2S2O3, dried over anhydrous Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography on silica gel using petroleum ether/EtOAc as the eluent to give the expected products 6aa as pale yellow solid, (80% yield).

As the paragraph descriping shows that 2879-20-1 is playing an increasingly important role.

Reference£º
Article; Lian, Mi; Li, Qi; Zhu, Yanping; Yin, Guodong; Wu, Anxin; Tetrahedron; vol. 68; 47; (2012); p. 9598 – 9605;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

29668-44-8, 2,3-Dihydrobenzo[b][1,4]dioxine-6-carbaldehyde is a benzodioxans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example-8Preparation of 2,3-dihydro-benzo[1,4]dioxin-6-yl-methylamine hydrochloride 242.0 g of Methanolic ammonia [as 100% w/w by chemical assay] [Note: as chemical assay: 23.0% w/w, volume 1350.0 ml] and 30.0 g (0.183 mol) of 1,4-benzodioxan-6-carboxaldehyde were charged into a 2.0 L 4 necked round bottom flask, connect to a mechanical stirrer, thermo meter socket and condenser at 20-30 C. Stirred the mass for 20-30 min at 20-30 C. After dissolution is clear. Reaction mass was charged into a 2.0 L hydrogenator kettle at 20-30 C. 30.0 g of Raney Nickel (with Methanol dried) was charged under nitrogen atmosphere. Kettle was fitted to the hydrogenator. Nitrogen atmosphere was removed in Hydrogenator kettle with hydrogen gas by slowly flushing. Hydrogen gas was feeded upto 50-55 psi in hydrogenation kettle under oscillation. Maintained the hydrogen gas pressure (50-55 psi) till the hydrogen gas consumption is stopped. Reaction mass temperature was raised to 40-45 C. After hydrogen gas consumption is stooped at 45-50 C. Reaction mass temperature was cooled to 25-30 C. Maintained the hydrogen gas pressure at 50-55 psi for till the hydrogen gas consumption is stopped (about 90-120 min) Raney nickel was filtered through hyflow bed under nitrogen atmosphere. Raney Nickel was washed with 300.0 ml of methanol under nitrogen atmosphere. Filterate was collected into a flask. Methanol was distilled completely under vacuum at mass temperature not crossing 55 C. Mass temperature was cooled to 40-45 C. and release the vacuum. 50.0 ml of isopropyl alcohol was added. Reaction mass pH was adjusted to 0.5+/-0.25 with IPA HCl. Maintained the mass temperature at 25-30 C. for 60-90 min under stirring. Solid was filtered and solid was washed with 20.0 ml of isopropyl alcohol. Compound was dried under vacuum at 40+/-5 C. Dry compound weight: 31.0 g (yield: 84.1%).Spectral data:FT-IR (K Br) (cm-1): 3447.6, 2977.6, 2870.0, 1594.5, 1506.6, 1474.0, 1285.8, 1077.7, 1051. 735.2, 617.9, 472.0MS: 202.6 [M+1]

The synthetic route of 29668-44-8 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Natco Pharma Limited; US2010/298351; (2010); A1;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

3663-80-7, 2,3-Dihydrobenzo[b][1,4]dioxine-2-carboxylic acid is a benzodioxans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Method I Ba (1 mmol) and 2,3-dihydrobenzo[b][1,4]dioxin-6-carboxylic acid (or 2,3-dihydrobenzo[b][1,4]dioxin-2-carboxylic acid) (1 mmol) together with EDCI (1.5 mmol) and HOBt (0.05 mmol) in CH2Cl2 (20 mL) were refluxed at room temperature for 10 h. While the reaction completed, the solution was washed with water for three times (30 mL each time). The remaining water layer was extracted by EtOAc for three times (30 mL each time). The organic layers (CH2Cl2 and EtOAc) were combined and then evaporated. The separated solid was crystallized from mixture of DMF and ethanol (9:1) to obtain the corresponding compound as translucent solid. 4.5.19 (2,3-Dihydrobenzo[b][1,4]dioxin-2-yl)(5-(4-methoxyphenyl)-3-phenyl-4,5-dihydro-1H-pyrazol-1-yl)methanone (D4) White crystal, mp: 104-106 ¡ãC. 1H NMR (CDCl3, 300 MHz) delta: 3.18-3.25 (d, J = 17.7 Hz, 1H), 3.68-3.75 (m, 1H), 3.77 (s, 3H), 4.33-4.39 (m, 1H), 4.57-4.62 (d, J = 11.4 Hz, 1H), 5.55-5.58 (m, 2H), 6.82-6.86 (m, 5H), 6.99-7.02 (m, 1H), 7.14-7.17 (d, J = 8.7 Hz, 2H), 7.43-7.46 (m, 3H), 7.73-7.77 (d, J = 7.5 Hz, 2H). MS (ESI): 415.16 (C25H23N2O4, [M+H]+). Anal. Calcd for C25H22N2O4: C, 72.45; H, 5.35; N, 6.76; O, 15.44. Found: C, 72.05; H, 5.34; N, 6.78.

As the paragraph descriping shows that 3663-80-7 is playing an increasingly important role.

Reference£º
Article; Yang, Yu-Shun; Li, Qing-Shan; Sun, Shuai; Zhang, Yan-Bin; Wang, Xiao-Liang; Zhang, Fei; Tang, Jian-Feng; Zhu, Hai-Liang; Bioorganic and Medicinal Chemistry; vol. 20; 20; (2012); p. 6048 – 6058;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

4442-53-9, 2,3-Dihydrobenzo[b][1,4]dioxine-5-carboxylic acid is a benzodioxans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: Method B: SOCl2 (10mL) was added to a stirred solution of compound 3 (20mmol) in anhydrous DMF (50mL). The reaction solution was allowed to stir at room temperature for approximately 4h. Then, active compound 4 (15mmol) and metronidazole (15mmol) were dissolved in CH2Cl2 followed by drop wise addition triethylamine and compound 5 was obtained with yield of 85percent. Compound 5 (10mmol), different substituted benzaldehydes (12mmol) and NaOH (15mmol) were dissolved in DMSO (30mL) at room temperature. The appropriate amount of water was then added in the residue and filtered. The resulting solid was collected and washed with cold water, dried and crystallized from anhydrous ethanol to get the desired compounds. All of the synthetic compounds gave satisfactory analytical and spectroscopic data, which were in full accordance with their depicted structures.

4442-53-9 2,3-Dihydrobenzo[b][1,4]dioxine-5-carboxylic acid 78184, abenzodioxans compound, is more and more widely used in various.

Reference£º
Article; Duan, Yong-Tao; Yao, Yong-Fang; Huang, Wei; Makawana, Jigar A.; Teraiya, Shashikant B.; Thumar, Nilesh J.; Tang, Dan-Jie; Tao, Xiang-Xiang; Wang, Zhong-Chang; Jiang, Ai-Qin; Zhu, Hai-Liang; Bioorganic and Medicinal Chemistry; vol. 22; 11; (2014); p. 2947 – 2954;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4442-54-0,2,3-Dihydro-1,4-benzodioxine-6-carboxylic acid,as a common compound, the synthetic route is as follows.

General procedure: 2,3-Dihydrobenzo[b][1,4]dioxin-6-carboxylic acid (or 2,3-dihydrobenzo[b][1,4]dioxin-2-carboxylic acid) (1 mmol) and 98percent H2SO4 (1 ml) in ethanol (20 mL) were refluxed at 80 ¡ãC for 5 h. While the reaction completed, 80percent hydrazine hydrate (2 mmol) was added and then the solution was refluxed at 80 ¡ãC for another 5 h. While the reaction completed, the ethanol was evaporated. The separated solid was filtered, washed with cold ethanol and dried to obtain white solid Bb.

The synthetic route of 4442-54-0 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Yang, Yu-Shun; Li, Qing-Shan; Sun, Shuai; Zhang, Yan-Bin; Wang, Xiao-Liang; Zhang, Fei; Tang, Jian-Feng; Zhu, Hai-Liang; Bioorganic and Medicinal Chemistry; vol. 20; 20; (2012); p. 6048 – 6058;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem