Introduction of a new synthetic route about 253-52-1

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

Phthalazine, cas is 253-52-1, it is a common heterocyclic compound, the phthalazine compound, its synthesis route is as follows.,253-52-1

General procedure: A solution of sodium azide (0.085 g, 1.3 mmol) in water (10 ml) was slowly added to the methanolic solution (15 ml) of Cd(NO3)24H2O (0.2 g, 0.65 mmol) and quinazoline (0.17 g, 1.30 mmol) and stirred at room temperature for 12 h. Light yellow crystalline precipitate of [Cd(Qnz)2(N3)2]n was collected in 70percent yield. The crystals suitable for X-ray structure determination were obtained by slow recrystallization from methanol

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

Reference£º
Article; Machura; Nawrot; Kruszynski; Dulski; Polyhedron; vol. 54; (2013); p. 272 – 284;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Introduction of a new synthetic route about Phthalazine

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

Phthalazine, cas is 253-52-1, it is a common heterocyclic compound, the phthalazine compound, its synthesis route is as follows.,253-52-1

General procedure: N-heteroarene (1 mmoL, 80 mg), alpha-keto acid (3 mmol), Formic acid (1 mmol, 38 muL), ammonium persulfate (3 mmoL, 685 mg), ferrous sulfate heptahydrate (0.08 mmoL, 22 mg) and 20 mL of mixed solvent (DCM: H2O = 3: 1) , 0.1 mL DMSO was added into a 25 mL round-bottomed flask. The mixture was stirred at 40 oC until TLC analysis indicating that the reaction was complete (witnessed by the disappearance of the N-heteroarene). After separation of organic phase, the residue was neutralized by 0.1 M sodium hydroxide solution, then extracted with DCM (3¡Á20 mL), combined the organic phases, dried over Na2SO4, and concentrated in vacuo. The residue was N-heteroarene (1 mmoL, 80 mg), alpha-keto acid (3 mmol), Formic acid (1 mmol, 38 muL), ammonium persulfate (3 mmoL, 685 mg), ferrous sulfate heptahydrate (0.08 mmoL, 22 mg) and 20 mL of mixed solvent (DCM: H2O = 3: 1) , 0.1 mL DMSO was added into a 25 mL round-bottomed flask. The mixture was stirred at 40 oC until TLC analysis indicating that the reaction was complete (witnessed by the disappearance of the N-heteroarene). After separation of organic phase, the residue was neutralized by 0.1 M sodium hydroxide solution, then extracted with DCM (3¡Á20 mL), combined the organic phases, dried over Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography on silica gel using a mixture of petroleum ether/EtOAc (v : v = 20 : 1) as eluent to afford the desired pure product.

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

Reference£º
Article; Wang, Xiu-Zhi; Zeng, Cheng-Chu; Tetrahedron; vol. 75; 10; (2019); p. 1425 – 1430;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Introduction of a new synthetic route about 253-52-1

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

Phthalazine, cas is 253-52-1, it is a common heterocyclic compound, the phthalazine compound, its synthesis route is as follows.,253-52-1

General procedure: Phthalazine (1) (91 mg, 0.70 mmol), 1,1-dicyanoalkene 2(0.70 mmol), and isocyanide 3 (0.70 mmol) were dissolvedin acetonitrile (1 ml). After that, distilled water(0.05?0.1 ml) was added to the reaction mixture up tovisible turbidity and stirred at 25?30¡ãC for 12?18 h. Thereaction mixture was evaporated to dryness and product 4was purified by crystallization from ethanol.

With the rapid development of chemical substances, we look forward to future research findings about 253-52-1

Reference£º
Article; Mironov, Maxim A.; Shulepov, Iliya D.; Kozhikhova, Ksenia V.; Ivantsova, Maria N.; Tokareva, Maria I.; Chemistry of Heterocyclic Compounds; vol. 53; 4; (2017); p. 430 – 433; Khim. Geterotsikl. Soedin.; vol. 53; 4; (2017); p. 430 – 433,4;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

New learning discoveries about 253-52-1

As the paragraph descriping shows that 253-52-1 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.253-52-1,Phthalazine,as a common compound, the synthetic route is as follows.

Phthalazine (1) (91 mg, 0.70 mmol), 1,1-dicyanoalkene 2(0.70 mmol), and isocyanide 3 (0.70 mmol) were dissolvedin acetonitrile (1 ml). After that, distilled water(0.05?0.1 ml) was added to the reaction mixture up tovisible turbidity and stirred at 25?30¡ãC for 12?18 h. Thereaction mixture was evaporated to dryness and product 4was purified by crystallization from ethanol. 3-(tert-Butylamino)-2-phenylpyrrolo[2,1-a]phthalazine-1-carbonitrile (4a). Reaction time 18 h. Yield 204 mg(86percent), pale-yellow crystals, mp 173?174¡ãC. IR spectrum,nu, cm?1: 3385 (NH), 3065, 2861 (CH), 2226 (CN), 1604,1486, 764, 729 (Ar). 1H NMR spectrum, delta, ppm (J, Hz):8.90 (1H, s, H-6); 8.75 (1H, d, J = 8.0, H-10); 8.05?7.25(8H, m, H Ar); 4.12 (1H, br. s, NH); 0.99 (9H, s, 3CH3).13C NMR spectrum, delta, ppm: 146.1 (=N); 134.4 (?NH);131.4 ( Ar); 129.8 ( Ar); 129.5 ( Ar); 129.1 ( Ar);128.8 ( Ar); 128.0 ( Ar); 126.1 ( Ar); 125.9 ( Ar);124.7 ( Ar); 122.5 ( Ar); 120.0 ( Ar); 116.2 ( Ar);112.7 (CN); 100.2 ( Ar); 55.4 ((CH3)3); 31.4 (CH3).Mass spectrum, m/z (Irel, percent): 340 [M]+ (17), 314 (12), 284(100), 222 (13), 206 (10), 168 (18), 129 (12), 56 (89).Found, percent: C 77.79; H 6.10; N 16.51. 22H20N4. Calculated, percent: C 77.62; H 5.92; N 16.46.

As the paragraph descriping shows that 253-52-1 is playing an increasingly important role.

Reference£º
Article; Mironov, Maxim A.; Shulepov, Iliya D.; Kozhikhova, Ksenia V.; Ivantsova, Maria N.; Tokareva, Maria I.; Chemistry of Heterocyclic Compounds; vol. 53; 4; (2017); p. 430 – 433; Khim. Geterotsikl. Soedin.; vol. 53; 4; (2017); p. 430 – 433,4;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Analyzing the synthesis route of 253-52-1

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.253-52-1,Phthalazine,as a common compound, the synthetic route is as follows.

General procedure: A solution of 2.00 g (15.0 mmol) of 2 in 20 mL of dry THF was cooled to 0 ¡ãC, and 8.0 mL of 2.0 M isopropylmagnesium chloride (3b) (16.0 mmol) in ether was slowly added dropwise over 20 min. The reaction was allowed to stir at 0 ¡ãC for 5 h and was then quenched with 50 mL of saturated NH4Cl and extracted with ethyl acetate (3 .x. 50 mL). The combined organic extracts were washed with saturated NaCl, dried (MgSO4), and concentrated under vacuum to give dihydrophthalazine 4b as a viscous, brown oil. This oil was dried under high vacuum for 30 min and was used without further purification.The crude 4b in dichloromethane at 0 ¡ãC was treated, as above, with 1.82 g (2.50 mL, 18.0 mmol) of triethylamine and 1.40 g (1.26 mL, 15.5 mmol) of 5, and the reaction was stirred for 2 h. Work-up and chromatography gave 1.83 g (40percent) of 6b as a viscous, brown oil.

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Nammalwar, Baskar; Bunce, Richard A.; Berlin, K. Darrell; Bourne, Christina R.; Bourne, Philip C.; Barrow, Esther W.; Barrow, William W.; European Journal of Medicinal Chemistry; vol. 54; (2012); p. 387 – 396;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Brief introduction of 253-52-1

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

253-52-1, Phthalazine is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Specific preparation methods are: no special protection, clean air to a single-necked flask were added sequentially magneton, phthalazine(52mg, 0.4mmol), was added sodium iodide (18mg, 30molpercent), 70percent of the mass fraction of the water phase of t-butyl hydroperoxide(152mg, 1.2mmol), then add toluene (728.8mg, 8mmol), toluene as both reactant and as a solvent, the reaction at 150 1Hours TLC showed the starting material is completely consumed phthalazine. Heating was stopped to quench the reaction. Without extraction, direct wetLoading, 200-300 mesh silica gel column chromatography, a mixed solvent of ethyl acetate and petroleum ether (1: 4) rinse. Separated structure of formula IXaFormula compound 84.0mg, 89percent yield;

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Xiangtan University; Yang, Luo; Luo, Wenkun; (17 pag.)CN105503724; (2016); A;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Downstream synthetic route of 253-52-1

As the paragraph descriping shows that 253-52-1 is playing an increasingly important role.

253-52-1, Phthalazine is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 1A1,2-phenylenedimethanamine[0168]Phthalazine (21.5 g, 0.165 mol), 10percent palladium on carbon (2 g), and methanol (125 mL) were combined in a pressure bottle and shaken at room temperature under 60 psi of hydrogen for 5 days. Raney-nickel? slurry (6.42 g) and 10percent palladium on carbon (0.50 g) were added, and the mixture was shaken at 50¡ã C. under 60 psi of hydrogen for 16 hours. The mixture was filtered through a nylon membrane and concentrated to give the titled compound: 1H NMR (300 MHz, DMSO-d6) delta ppm 7.32 (dd, J=5.4, 3.5 Hz, 2H), 7.17 (dd, J=5.6, 3.4 Hz, 2H), 3.74 (s, 4H); MS (DCI/NH3) m/z 137 (M+H)+.

As the paragraph descriping shows that 253-52-1 is playing an increasingly important role.

Reference£º
Patent; AbbVie Inc.; Cowart, Marlon D.; Liu, Huaqing; Altenbach, Robert; US2013/40940; (2013); A1;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

 

Analyzing the synthesis route of 253-52-1

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.253-52-1,Phthalazine,as a common compound, the synthetic route is as follows.

A solution of 3.0g (23.3mmol) of phthalazine in 20mL of concentrated sulfuric acid was brought to 100¡ãC. To the phthalazine solution was added portion-wise 18.8g (186mmol) of potassium nitrate over 1-h time period. After 72h at 100¡ãC, the solution was cooled to room temperature, poured over ice, and neutralized with ammonium hydroxide to produce a yellow-tan precipitate. The precipitate was collected and dried to afford 2.3g (56percent) of the 5-nitrophthalazine intermediate as a light yellow solid. 1H NMR (400MHz, DMSO-d6) delta: 10.2 (s, 1 H), 9.98 (s, 1 H), 8.84 (d, J=7.4Hz, 1H), 8.59 (d, J=7.6Hz, 1H), 8.20 (dd, J=7.4, 14.9Hz, 1H). 13C NMR (100.17MHz, DMSO-d6) delta: 152.1, 146.3, 141.0, 133.2, 131.8, 130.0, 127.4, 118.7.

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Paige, Mikell; Kosturko, George; Bulut, Gu?llay; Miessau, Matthew; Rahim, Said; Toretsky, Jeffrey A.; Brown, Milton L.; U?ren, Aykut; Bioorganic and Medicinal Chemistry; vol. 22; 1; (2014); p. 478 – 487;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Analyzing the synthesis route of 253-52-1

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.253-52-1,Phthalazine,as a common compound, the synthetic route is as follows.

General procedure: N-heteroarene (1 mmoL, 80 mg), alpha-keto acid (3 mmol), Formic acid (1 mmol, 38 muL), ammonium persulfate (3 mmoL, 685 mg), ferrous sulfate heptahydrate (0.08 mmoL, 22 mg) and 20 mL of mixed solvent (DCM: H2O = 3: 1) , 0.1 mL DMSO was added into a 25 mL round-bottomed flask. The mixture was stirred at 40 oC until TLC analysis indicating that the reaction was complete (witnessed by the disappearance of the N-heteroarene). After separation of organic phase, the residue was neutralized by 0.1 M sodium hydroxide solution, then extracted with DCM (3¡Á20 mL), combined the organic phases, dried over Na2SO4, and concentrated in vacuo. The residue was N-heteroarene (1 mmoL, 80 mg), alpha-keto acid (3 mmol), Formic acid (1 mmol, 38 muL), ammonium persulfate (3 mmoL, 685 mg), ferrous sulfate heptahydrate (0.08 mmoL, 22 mg) and 20 mL of mixed solvent (DCM: H2O = 3: 1) , 0.1 mL DMSO was added into a 25 mL round-bottomed flask. The mixture was stirred at 40 oC until TLC analysis indicating that the reaction was complete (witnessed by the disappearance of the N-heteroarene). After separation of organic phase, the residue was neutralized by 0.1 M sodium hydroxide solution, then extracted with DCM (3¡Á20 mL), combined the organic phases, dried over Na2SO4, and concentrated in vacuo. The residue was purified by column chromatography on silica gel using a mixture of petroleum ether/EtOAc (v : v = 20 : 1) as eluent to afford the desired pure product.

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Wang, Xiu-Zhi; Zeng, Cheng-Chu; Tetrahedron; vol. 75; 10; (2019); p. 1425 – 1430;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem

Brief introduction of 253-52-1

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

253-52-1, Phthalazine is a phthalazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: Phthalazine (1) (91 mg, 0.70 mmol), 1,1-dicyanoalkene 2(0.70 mmol), and isocyanide 3 (0.70 mmol) were dissolvedin acetonitrile (1 ml). After that, distilled water(0.05?0.1 ml) was added to the reaction mixture up tovisible turbidity and stirred at 25?30¡ãC for 12?18 h. Thereaction mixture was evaporated to dryness and product 4was purified by crystallization from ethanol.

The synthetic route of 253-52-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Mironov, Maxim A.; Shulepov, Iliya D.; Kozhikhova, Ksenia V.; Ivantsova, Maria N.; Tokareva, Maria I.; Chemistry of Heterocyclic Compounds; vol. 53; 4; (2017); p. 430 – 433; Khim. Geterotsikl. Soedin.; vol. 53; 4; (2017); p. 430 – 433,4;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem