Category: 1015-89-0

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. 1015-89-0, name is Phenanthridin-6(5H)-one, A new synthetic method of this compound is introduced below., Quality Control of Phenanthridin-6(5H)-one

The 5,6-dihydro-phenanthridine (Ik) was prepared using the following procedure: Into a 500 mL round bottom flask equipped with a magnetic stir bar and a reflux condensor was placed 6(5H)-Phenanthridinone (1000 mg, 5123 mumol), THF (250 mL) (fine suspension). The flask is sparged with nitrogen, 2M BH3-dimethylsulfide complex in THF (10 mL) is added. This is allowed to stir at reflux for 24 hours. TLC shows reaction still incomplete (1/1, ethyl acetate/heptane). Solvents removed under reduced pressure. Water (50 mL) and ethyl acetate (100 mL) added. The aqueous layer is separated with ethyl acetate (3 x 100 mL). The organic layers are combined, dried(sodium sulfate), solids removed by filtration, and the solvents removed under reduced pressure. This is purified by silica column chromatography using heptane to 50percent ethylacetate in heptane. The best fractions are pooled and the solvents are removed under reduced pressure to afford an off-white solid (270 mg, Yield: 29percent). LC-MS shows mass 182 (M+H)+.

The synthetic route of 1015-89-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TIBOTEC PHARMACEUTICALS LTD.; MEDIVIR AB; WO2008/96001; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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 1015-89-0 as follows. 1015-89-0

(ii) BDS, THF, reflux, 24 h; (yield 20percent)

According to the analysis of related databases, 1015-89-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ROBERTS, Edward; MITTAPALLI, Gopi Kumar; VELLUCCI, Danielle; YANG, Jun; GUERRERO, Miguel; URBANO, Mariangela; ROSEN, Hugh; WO2014/116684; (2014); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 1015-89-0, name is Phenanthridin-6(5H)-one, A new synthetic method of this compound is introduced below., SDS of cas: 1015-89-0

The 5,6-dihydro-phenanthridine (Ik) was prepared using the following procedure: Into a 500 mL round bottom flask equipped with a magnetic stir bar and a reflux condensor was placed 6(5H)-Phenanthridinone (1000 mg, 5123 mumol), THF (250 mL) (fine suspension). The flask is sparged with nitrogen, 2M BH3-dimethylsulfide complex in THF (10 mL) is added. This is allowed to stir at reflux for 24 hours. TLC shows reaction still incomplete (1/1, ethyl acetate/heptane). Solvents removed under reduced pressure. Water (50 mL) and ethyl acetate (100 mL) added. The aqueous layer is separated with ethyl acetate (3 x 100 mL). The organic layers are combined, dried(sodium sulfate), solids removed by filtration, and the solvents removed under reduced pressure. This is purified by silica column chromatography using heptane to 50percent ethylacetate in heptane. The best fractions are pooled and the solvents are removed under reduced pressure to afford an off-white solid (270 mg, Yield: 29percent). LC-MS shows mass 182 (M+H)+.

The synthetic route of 1015-89-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TIBOTEC PHARMACEUTICALS LTD.; MEDIVIR AB; WO2008/96001; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 1015-89-0, These common heterocyclic compound, 1015-89-0, name is Phenanthridin-6(5H)-one, 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.

Phenanthridin-6(5H)-one (1; 0.100 g, 0.492 mmol) was placed in aSchlenk flask under argon. POCl3 (3.29 g, 2 mL, 21.4 mmol, 43 equiv)was added, and the mixture was stirred at 100 C for 24 h. The mixturewas cooled, poured onto ice, and stirred for 15 min. The solidthat formed was collected by filtration, washed thoroughly with H2O,and dried in vacuum to give a light-brown solid; yield: 95.5 mg (87%);Rf = 0.65 (hexane-EtOAc, 5:1; detection: UV).IR (KBr): 3103, 3072, 3039, 1613, 1574, 757 cm-1.1H NMR (600 MHz, acetone-d6): delta = 7.69 (ddd, J = 8.2, 7.0, 1.4 Hz, 1 H,H-12), 7.75 (ddd, J = 8.2, 7.0, 1.5 Hz, 1 H, H-13), 7.77 (ddd, J = 8.2, 7.0,1.2 Hz, 1 H, H-4), 7.91 (ddd, J = 8.3, 7.0, 1.3 Hz, 1 H, H-5), 8.10 (ddd,J = 8.2, 1.4, 0.6 Hz, 1 H, H-14), 8.48 (ddd, J = 8.2, 1.3, 0.6 Hz, 1 H, H-3),8.54 (ddt, J = 8.3, 1.5, 0.6 Hz, 1 H, H-11), 8.62 (ddt, J = 8.3, 1.2, 0.3 Hz, 1H, H-6).13C NMR (151 MHz, acetone-d6): delta = 151.45 (C-2), 143.31 (C-8),134.51 (C-10), 131.77 (C-5), 129.36 (C-13), 129.32 (C-14), 128.25 (C-4), 127.74 (C-3), 127.49 (C-12), 124.90 (C-9), 124.03 (C-7), 122.28 (C-6), 122.21 (C-11). MS (ESI): m/z (%) = 214.1 [M + H]+ (100).HRMS (ESI): m/z [M + H]+ calcd for C13H9ClN: 214.0148; found:214.0149.

Statistics shows that Phenanthridin-6(5H)-one is playing an increasingly important role. we look forward to future research findings about 1015-89-0.

Reference:
Article; Sonawane, Manoj R.; Vavra, Jan; ?aman, David; Cisa?ova, Ivana; Teply, Filip; Synthesis; vol. 47; 22; (2015); p. 3479 – 3488;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1015-89-0, name is Phenanthridin-6(5H)-one, belongs to amides-buliding-blocks compound, 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 1015-89-0, Computed Properties of C13H9NO

Step 1: Synthesis of 2-bromophenanthridone 99.8 g (511 mmol) was added to the phenanthridine dinon 3 ? flask equipped with a plurality of necked stirring arm and is equipped with a condenser. It was added to 1.2 ? of glacial acetic acid and the mixture was stirred at 150 rpm, heated to reflux. A 90 g (562 mmol) Br2 dispersed in 100 acetic acid was added dropwise over 3 hours to a solution being refluxed. After the addition, the mixture was found to be analyzed is about 80% complete. Based on this analysis, it was added dropwise while refluxing the (in the 30 acid) Add 20 g of Br2 in the mixture. After the addition, the analysis is> 90% completed. It was added dropwise to 20 g Br2 end (30 of the acid) and the mixture was stirred for 1 hour after addition. Final analysis> was 97%. The mixture was cooled, water was added in 1 ?, and the mixture was filtered. By stirring in a wet solids aqueous solution of sodium thiosulfate was decomposed the residual bromine, and filtered again. thisRinse the solid with H2O, and allowed to dry under vacuum to remove residual water. Thereafter, the solid was recrystallized from nitrobenzene (> ? 2), and collected on a funnel to give 128 g of 2-bromo-phenanthridine dinon (90.8% yield).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; UNIVERSAL DISPLAY CORPORATION; NOLIS, DAVID B; LIN, CHOOK; MCKINSEY, PETER BODON; CHAI, CHUI LEE; WALTERS, ROBERT W; PIERS, SCOTT A; BROWN, CORY S; IGOR, WALTER H; (101 pag.)KR2016/30582; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 1015-89-0, A common heterocyclic compound, 1015-89-0, name is Phenanthridin-6(5H)-one, molecular formula is C13H9NO, 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.

EXAMPLE 28 STR46 To a mixture of phenanthridone 32 and PCl5 is added a molar excess of POCl3. The reaction is heated to reflux until chromatographic analysis indicates complete reaction, cooled and quenched by pouring onto ice. The aqueous layer is extracted with CHCl3. The organic layer is dried over MgSO4, filtered and evaporated to provide phenanthridine 33.

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; Merck & Co., Inc.; US5336674; (1994); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Reference of 1015-89-0, 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 1015-89-0 as follows.

Phenanthridin-6(5H)-one (1; 1.017 g, 5.209 mmol) was placed in aSchlenk flask under argon. Freshly distilled CH2Cl2 (30 mL) was added,and the resulting solution was cooled to 0 C. Tf2O (3.00 g, 1.74 mL,10.6 mmol, 2.0 equiv) was added dropwise to the suspension. After40 min, the mixture became almost completely homogeneous. After afurther 20 min of stirring, pyridine (0.414 g, 423 muL, 5.233 mmol, 1.02equiv) was slowly added and a precipitate formed. The resulting mixturewas stirred at 0 C for 40 min. Next, H2O (20 mL) was added andthe mixture was extracted with CH2Cl2 (2 ¡Á 30 mL). The organic layerwas dried (Na2SO4), filtered, and concentrated on a rotary evaporator.The resulting residue was dissolved in Et2O (10 mL) and hexane (60mL) was added. Most of the volatiles were then slowly removed on arotary evaporator. The resulting suspension was filtered to give abeige solid; 1.551 g (91%); mp 82-83 C (Et2O-hexane); Rf = 0.57(hexane-EtOAc, 5:1).IR (CHCl3): 3082, 3047, 1629, 1615, 1467, 1426, 1244, 1216, 1137,1023, 607 cm-1.1H NMR (600 MHz, acetone-d6): delta = 9.00 (ddt, J = 8.3, 1.1, 0.6 Hz, 1 H,H-6), 8.89 (ddt, J = 8.1, 1.4, 0.6 Hz, 1 H, H-11), 8.34 (ddd, J = 8.3, 1.4,0.7 Hz, 1 H, H-3), 8.19 (ddd, J = 8.3, 7.1, 1.4 Hz, 1 H, H-5), 8.11 (ddd,J = 8.0, 1.5, 0.7 Hz, 1 H, H-14), 8.02 (ddd, J = 8.3, 7.1, 1.1 Hz, 1 H, H-4),7.94 (ddd, J = 8.0, 7.1, 1.4 Hz, 1 H, H-13), 7.90 (ddd, J = 8.1, 7.1, 1.5 Hz,1 H, H-12).13C NMR (151 MHz, acetone-d6): delta = 152.50 (C-2), 141.70 (C-8),137.27 (C-10), 134.08 (C-5), 130.96 (C-13), 130.10 (C-4), 129.92 (C-14), 129.35 (C-12), 125.53 (C-7), 124.73 (C-3), 124.02 (C-6), 123.93(C-11), 119.50 (q, JC-F = 320 Hz, CF3), 119.10 (C-9).MS (ESI): m/z (%) = 350.1 [M + Na]+ (100).HRMS (ESI): m/z [M + H]+ calcd for C14H9F3NO3S: 328.0250; found:328.0250.

According to the analysis of related databases, 1015-89-0, the application of this compound in the production field has become more and more popular.

Reference:
Article; Sonawane, Manoj R.; Vavra, Jan; ?aman, David; Cisa?ova, Ivana; Teply, Filip; Synthesis; vol. 47; 22; (2015); p. 3479 – 3488;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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 1015-89-0 as follows. 1015-89-0

(ii) BDS, THF, reflux, 24 h; (yield 20percent)

According to the analysis of related databases, 1015-89-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ROBERTS, Edward; MITTAPALLI, Gopi Kumar; VELLUCCI, Danielle; YANG, Jun; GUERRERO, Miguel; URBANO, Mariangela; ROSEN, Hugh; WO2014/116684; (2014); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics